Method and device for preparing compositions rich in episesamin |
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IPC classes for russian patent Method and device for preparing compositions rich in episesamin (RU 2408598):
   
 Method for synthesis of 4beta-amino-4'-demethyl-4-desoxypodophyllotoxin / 2405787
Invention relates to a method for synthesis of 4β-amino-4'-demetyl-4-desoxypodophyllotoxin of formula (1), involving the following steps: a) reaction of thiourea and 4β-halogenoacetamido-4'-demethyl-4-desoxypodophyllotoxin in a medium of a weak pure acid or mixture of acid, water an organic solvent without using any other solvent at temperature higher than ambient temperature; b) extraction of 4β-amino-4'-demethyl-4- desoxypodophyllotoxin.
 Pest control agent / 2405310
Invention describes compositions for use as a pest control agents containing a compound of formula (I), or a salt of the said compound, acceptable in agriculture or horticulture, as an active ingredient or carrier which is acceptable in agriculture or horticulture:
 Method for synthesis of epothilone derivatives, novel epothilone derivatives, as well as novel intermediate compounds for realising said method and synthesis methods thereof / 2404985
Invention relates to novel epothilone derivatives of formula (8)
 Dibenzylidene sorbitol (dbs) based compounds, composition and method of using said compounds / 2401271
Invention relates to novel dibenzylidene sorbitol (DBS) compounds of formula 1:
 Tricyclic compounds of benzopyran as antiarrhythmic agents / 2380370
Invention relates to benzopyran derivatives of formula
![Method for production of (3r, 3as,6ar)-hexahydrofuro[2,3-b]furan-3-yl(1s,2r)-3-[[(4-aminophenyl)sulfonyl](isobutyl)amino]-1- benzyl-2-hydroxypropylurethane](http://img.russianpatents.com/img_data/1042/10421867-s.gif) Method for production of (3r, 3as,6ar)-hexahydrofuro[2,3-b]furan-3-yl(1s,2r)-3-[[(4-aminophenyl)sulfonyl](isobutyl)amino]-1- benzyl-2-hydroxypropylurethane / 2376308
Production of (3R,3aS,6aR)-hexahydrofuro[2,3-b]furan-3-yl(1S,2R)-3-[[(4-aminophenyl)sulfonyl](isobutyl)amino]-1-benzyl-2-hydroxypropylurethane is carried out with application of intermediate compound 4-amino-N-[(2R,3S)-3-amino-2-hydroxy-4-phenylbutyl]-N-(isobutyl)benzenesulfonamide. (3R,3aS,6aR)- hexahydrofuro [2,3-b]furan-3-yl(1S,2R)-3-[[(4-aminophenyl)sulfonyl](isobutyl)amino]-1-benzyl-2-hydroxypropylurethane is applicable, in particular as inhibitor of HIV protease.
 Derivatives of 2-(hereto)aryl-substituted tetrahydroquinolines / 2375354
There are presented compounds of formula I
 Method of polyolefin composition nucleation by acetal compounds / 2348637
Invention concerns method of polyolefin composition nucleation by mixing the composition with compound of the structural formula:
 Method of obtaining epotilone derivatives / 2343155
Method ensures carrying out aldole condensation in presence of epoxide mesilate and tosilate, using auxiliary chiral sultamic group as carboxyl- protecting group, as a result, reduction and oxidation stages, requiring extra time, before carrying out final stage of macrolactonisation are excluded. Introduction of epoxidic group at early stages of method allows also excluding stage of epoxilation of more complex intermediate compounds at further stages of process.
 New tetracyclic compounds containing heteroatom, used as selective modulators of oestrogen receptors / 2331645
Invention pertains to new tetracyclic compounds containing a heteroatom. The compounds can be used in treating and/or prevention of disorders, associated with oestrogen depletion, such as hot flash, vaginal dryness, osteopenia and osteoporosis; sensitive cancerous diseases hormone and hyperplasia of the lacteal gland, endometrium, cervix uteri and prostate; endometriosis, uterus fibrosis and osteoarthritis, and as contraceptive agents, used either separately or combined with progestogen or a progestogen antagonist.
 Fixed bed reactor and method for synthesis of 2,2-bis(4-hydroxyphenyl)propane using said reactor / 2404153
Phenol and acetone mixture is fed into the reactor through a liquid distributor 1 and brought into contact with a catalyst bed from an ion-exchange resin 2. After passing through inlet pipes 3, the liquid product is collected using a liquid collection pipe 4. The ready product comes out of the reactor system trough a liquid outlet pipe 5.
Caprolactam synthesis method / 2403239
Present invention relates to a method for synthesis of caprolactam from alkylcyanovalerate which involves bringing alkylcyanovalerate into contact with hydrogen in gaseous state in the presence of a hydrogenation catalyst and a ring formation catalyst, and treatment after condensation of a gaseous stream containing the formed lactam in order to separate ammonium which may be present, the formed alcohol and/or the caprolactam solvent and extraction of caprolactam, where the hydrogenation catalyst includes a metal element or a mixture of metal elements selected from a group containing an active metal element in form of iron, ruthenium, rhodium, iridium, palladium, cobalt, nickel, chromium, osmium and platinum or several metals from this list, and the ring formation catalyst is porous aluminium oxide.
 Method of obtaining acrolein or acrylic acid or mixture thereof from propane / 2391330
In accordance with the method A) at least two propane-containing gas supply streams are fed into the first reaction zone A, where at least one of the said streams contains fresh propane, and propane fed into this reaction zone undergoes heterogeneous catalytic dehydrogenation with a fixed bed catalyst, obtaining a propane- and propylene-containing gaseous mixture of products A, B) which is extracted from reaction zone A, in the first separation zone, A is separated from at least a portion of components contained in it, which are different from propane and propylene, and the remaining gaseous mixture of products A' which contains propane and propylene C) is used in the second reaction zone B for supplying at least one oxidation reactor, and propylene contained in the gaseous mixture of products A' in at least one oxidation reactor undergoes heterogeneous catalytic two-step gas-phase partial oxidation with molecular oxygen to acrylic acid or a mixture of acrolein and acrylic acid as an end product, as well as to an excess molecular oxygen-containing gaseous mixture of products B, D) which is extracted from the reaction zone B, in the second separation zone B, the end product contained in it is extracted through absorption or fractional condensation, and at least a portion of the remaining residual gas which contains unconverted propane, molecular oxygen, and also if necessary, unconverted propylene are recycled into the reaction zone A as at least one of two propane-containing supply streams, where the said recycling into the reaction zone A is done along the path of the heterogeneous catalysed dehydrogation of propane in that reaction zone such that, at the point for feeding the recycled gas into reaction zone A at least 5 mol % of propane has already undergone dehydrogenation, where the said propane is fed into this reaction zone with other supply streams, where molar ratio of the propylene contained in the reaction gaseous mixture to molecular hydrogen contained in the said mixture within the reaction zone A does not exceed 10.
 Method of preparing salt compound (4,5-dihydroisoxazol-3-yl)thiocarboxamidine / 2378261
Invention relates to a method of preparing a salt compound (4,5-dihydroisoxazol-3-yl)thiocarboxamidine of formula (2)
 Method of producing liquid composition, containing hyperpolarised 13c-pyruvate, composition containing hyperpolarised 13c-pyruvate (versions), use thereof (versions), radical and use thereof / 2374252
Invention relates to a method of producing a liquid composition which contains hyperpolarised 13C-pyruvate, involving: a) formation of a liquid mixture containing a radical of formula (I)
 Stepped counterflow catalystic oxidation of disubstituted benzene / 2374219
Invention relates to a continuous stepped counterflow method of catalytic oxidation in a solvent of at least one benzene compound, containing two substituting groups, which are selected from alkyl, hydroxyalkyl, aldehyde, carboxyl groups and their mixtures, which can be oxidised to the corresponding acid derivative, involving the following steps: (a) introducing a mixture of material into the first oxidation step, containing at least part of the total amount of each of: (i) solvent, which is an organic acid, (ii) at least one catalytically active metal, selected from manganese, cobalt, nickel, zirconium, hafnium, cerium and their mixtures, and (iii) bromine in molar ratio, in terms of all catalytically active metals, in the interval from 1:20 to 5:1 and from 7 to 60 wt % of the total amount of at least one disubstituted benzene, introduced at steps (a) and (d); (b) partial oxidation of at least one disubstituted benzene at the first oxidation step in the presence of a gas, containing molecular oxygen initially in amount of 3 to 20 vol. %, at temperature ranging from 121°C to 205°C and relative quantities of disubstituted benzene, catalytic metal, solvent and bromine, introduced at step (a), so that from 25 to 99.95 wt % disubstituted benzene, added at the first oxidation step, is oxidised with formation of a gaseous mixture, containing unreacted molecular oxygen, evaporated solvent and a first mixture of products, containing acid derivative, partially oxidised disubstituted benzene, unreacted disubstituted benzene and solvent, and at pressure from 8.96·105 to 14.8·105 Pa, sufficient for keeping disubstituted benzene, partially oxidised disubstituted benzene, acid derivative and solvent in liquid state or in form of a suspension of solid substance in a liquid, so that concentration of residual molecular oxygen in the remaining gaseous mixture ranges from 0.3 to 2 vol. %; (c) extraction of the obtained first product mixture after the first oxidation step and supplying at least part of the extracted first product mixture to the second oxidation step; (d) supplying gas to the second oxidation step, containing molecular oxygen and residue form total amount of disubstituted benzene, catalytic metal, solvent and bromine; (e) oxidation at the second oxidation step of partially oxidised disubstituted benzene and unreacted disubstituted benzene, supplied to the second oxidation step, with a gas containing molecular oxygen in amount of 15 to 50 vol. %, at temperature ranging from 175°C to 216°C and relative quantities of disubstituted benzene, partially oxidised disubstituted benzene, catalytic metal, solvent and bromine, introduced at step (a), so that from 96 to 100 wt % disubstituted benzene and partially oxidised disubstituted benzene is oxidised with formation of a gaseous mixture, which contains unreacted molecular oxygen, evaporated solvent and a second product mixture, containing acid derivative and solvent, and at pressure from 11.7·105 to 16.2·105 Pa so as to keep the acid derivative, partially oxidised disubstituted benzene and unreacted disubstituted benzene mainly in liquid state or in form of a suspension of solid substance in a liquid, so that concentration of residual molecular oxygen in the remaining gaseous mixture ranges from 3 to 15 vol. %; (f) extraction after the second oxidation step of the second product mixture, containing acid derivative; and (g) tapping gas which contains residual molecular oxygen after the second oxidation step and returning it to the first oxidation step.
 Method of removing iron containing pollutant substances from liquid streams during production and/or cleaning of aromatic acids / 2326105
Invention pertains to the perfection of the method of regulating quantities of dissolved iron in liquid streams during the process of obtaining aromatic carboxylic acids or in the process of cleaning technical aromatic carboxylic acids, characterised by that, to at least, part of the liquid stream for regulating the quantity of dissolved iron in it, at least one peroxide with formula R1-O-O-R2 is added. Here R1 and R2 can be the same or different. They represent hydrogen or a hydrocarbon group, in quantities sufficient for precipitation of the dissolved iron from the liquid. The invention also relates to the perfection of the method of obtaining an aromatic carboxylic acid, through the following stages: A) contacting the crude aromatic material which can be oxidised, with molecular oxygen in the presence of an oxidising catalyst, containing at least, one metal with atomic number from 21 to 82, and a solvent in the form of C2-C5 aliphatic carboxylic acid in a liquid phase reaction mixture in a reactor under conditions of oxidation with formation of a solid product. The product contains technical aromatic carboxylic acid, liquid, containing a solvent and water, and an off-gas, containing water vapour and vapour of the solvent; B) separation of the solid product, containing technical aromatic carboxylic acid from the liquid; C) distillation of at least part of the off gas in a distillation column, equipped with reflux, for separating vapour of the solvent from water vapour. A liquid then forms, containing the solvent, and in the upper distillation cut, containing water vapour; D) returning of at least, part of the liquid from stage B into the reactor; E) dissolution of at least, part of the separated solid product, containing technical aromatic carboxylic acid, in a solvent from the cleaning stage with obtaining of a liquid solution of the cleaning stage; F) contacting the solution from the cleaning stage with hydrogen in the presence of a hydrogenation catalyst and under hydrogenation conditions, sufficient for formation of a solution, containing cleaned aromatic carboxylic acid, and liquid, containing a cleaning solvent; G) separation of the cleaned aromatic carboxylic acid from the solution, containing the cleaning solvent, which is obtained from stage E, with obtaining of solid cleaned aromatic carboxylic acid and a stock solution from the cleaning stage; H) retuning of at least, part of the stock solution from the cleaning stage, to at least, one of the stages B and E; I) addition of at least, one peroxide with formula R1-O-O-R2, where R1 and R2 can be the same or different, and represent hydrogen or a hydrocarbon group, in a liquid from at least one of the other stages, or obtained as a result from at least one of these stages, to which the peroxide is added, in a quantity sufficient for precipitation of iron from the liquid.
Method and system for olefin epoxydation / 2296126
Claimed method includes interaction of raw materials containing olefin, oxygen and reaction modifying agent in presence high selective silver-based catalyst at reaction temperature of T. Relative amount of reaction modifying agent is Q, wherein Q is ratio of effective molar amount of active sites of reaction modifying agent representing in raw materials to effective molar amount of hydrocarbon representing in raw materials. Epoxydation process is carried out in the first process phase wherein T=T1 and Q=Q1. Further process is carried out in the second process phase at T=T2 and Q=Q2, wherein T2 and Q2 are differ from T1 and Q1. Q2 is calculated according to equation Q2 = Q1 + B(T2 - T1) wherein B represents constant more than 0. Also disclosed are method for production of 1,2-diol or 1,2-diol ether; reaction system used in investigation; computer program product for calculations and computer system including said program product and information processing system.
 Method for finding ligands / 2295518
Invention relates to a conjugate target - compound chosen from the following group:
Method and systems for epoxidation of olefin / 2294327
Invention relates to a method for the epoxidation reaction of olefin. Method involves interaction of the parent olefin-containing raw, oxygen and an agent modifying reaction in the presence of a silver-base catalyst. Agent modifying the reaction presents in the relative amount Q that represents the ratio of effective molar amount of active parts of reaction modifying agent presenting in the parent raw to the effective molar amount of hydrocarbons presenting in the parent raw. Proposed method involves the following steps: interaction in the first stage of process wherein Q values are equal to Q1 and the following interaction in the second step of process wherein the composition of the parent raw differs from composition of the parent raw used in the first step of process and Q value is equal to Q2 wherein value Q2/Q1 = 0.5-1.5. Also, invention relates to a method for synthesis of 1,2-diol or 1,2-diol ether, system for realization of method, the end product and a computer system suitable for using with proposed method.
 Stereoselective method of obtaining fluorinated chiral molecule / 2389717
Invention relates to a stereoselective method of obtaining a fluorinated molecule having a fluorine atom with asymmetrical carbon (R) or (S) configuration in the α position relative an ester or ketone group in which: (i) a fluorosulphite compound of given configuration on C* which carries the fluorosulphite group of formula (III)
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FIELD: chemistry. SUBSTANCE: sesamin or sesamin-containing composition undergoes epimerisation in such a way that a portion of the sesamin converts to episesamin. Episesamin is crystallised through recrystallisation. The device for producing sesamin has an isomerisation unit which has a mixing reservoir for mixing oil or fat containing sesamin or a sesamin-containing composition with an acid catalyst; a crystallisation unit having a crystallisation reservoir for carrying out recrystallisation; a liquid supply line which connects the mixing reservoir with the crystallisation reservoir. EFFECT: high output of product. 21 cl, 2 dwg, 5 ex, 3 tbl
The technical field The invention relates to a method and apparatus for obtaining compositions enriched epistemical that contain epistemic in concentrations of more than 50 wt.%, more specifically this invention relates to a method and apparatus for obtaining compositions enriched epistemical that contain epistemic in quantities of more than 50 wt.%, preferably 60 wt.% or higher, more preferably 70 wt.% and above epimerize of sesamin or staminodial composition in such a way that as a result of epimerization of stamina obtain a mixture enriched epistemical, sesamin and epistemological mixture, and then carry out the recrystallization Ameritania mixture of epistemon, stamina. The level of technology Epistemon is stereoisomerism stamina. More precisely, sesamin is an optically active compound having a structure represented by the formula I: [Formula 1]
and epistemon, the isomer of stamina, is an optically active compound having a structure represented by formula II: [Formula 2]
It is obvious that of the two formulas of sesamin has a symmetric structure on the plane, and epistemon, by contrast, has an asymmetric structure. Sesamin is one them of the basic compounds Lignano sesame seeds and is contained in the seeds sesame seeds in quantities of 0.1-0.5%. In contrast, epistemic does not occur in nature in sesame seeds, but when the sesame oil pressing at the stage of refining in obtaining oil for salad greater purity and similar sesamin undergoes epimerization with the formation of epistemon as a by-product (reference to non-patent literature 1), and, as you know, sesamine allocated from refined sesame oil, contain sesamin and epistemic in a ratio of about 1:1 by weight (reference to non-patent literature 2). Experiments with mixtures of stamina and epistemon (approximately 1:1) showed different physiological activity of Stamenov, including, for example, the inhibitory activity for Δ5-saturas (links to non-patent literature 3 and 4, and a link to a patent (1), an antioxidant for lipids (reference patent 2 and 3), antihypertensive (reference to patent 4), action aimed at the improvement of liver functions (reference to patent 5), action aimed at the elimination of active oxygen (reference to patent 6), action on the reduction of cholesterol in the blood and/or hypocholesterolemic action (links to patents 7 and 8), the effect of in vivo stabilization of high molecular weight unsaturated fatty acid (reference to patent 9) and action aimed at preventing diseases, also decided the Lenna alcohol dependence (reference to patent 10). Recent studies have also revealed differences in the physiological activities of stamina and epistemon. For example, it was shown that when administered orally to rats mixtures of stamina and epistemon (approximately 1:1) localization in vivo such that the flow of epistemon authorities at least twice more intense than stamina (reference to non-patent literature 5). In addition, in experiments in which rats orally was administered separately sesamin and epistemon, results were obtained, showing that epistemic significantly increases the gene expression and enzymatic activity of the enzymes of β-oxidation in the liver compared with sesamin and that there is no difference in the activities of stamina and epistemon in relation to inhibition of fatty acid synthase (reference to non-patent literature 6). These data have recently been presented in several works concerning the useful properties of epistemon. Currently proposed methods of production lignana sesame include the extraction of sesame oil organic solvents, such as alcohol (e.g. methanol, acetone, petroleum ether and acetonitrile, or mixtures of these solvents with water, as well as molecular distillation sesame oil (reference to non-patent literature 11). [Reference patent 1] official Gazette of JP 3-27319 A [Link n the patent 2] official Gazette of JP 5-051388 A [Link to patent 3] official Gazette of JP 2001-139579 A [Link to patent 4] official Gazette of JP 8-268887 A [Link to patent 5] official Gazette of JP 4-099331 A [Link to patent 6] official Gazette of JP 6-227977 A [Link to the patent 7] the official newsletter of the Japan patent No. 3001589 [Link to patent 8] official Gazette of JP 4-159221 A [Link to patent 9] official Gazette of JP 11-269456 A [Link to patent 10] the official newsletter of the Japan patent No. 3124062 [Link to patent 11] official Gazette of JP 10-120695 A [Link to non-patent literature 1] Namiki et al., “Goma - Sono Called to Kinousei (Sesame - Its Science and Functions)”, Maruzen Planet Co., Ltd. (1998) [Link to non-patent literature 2] Fukuda, Y. et al., J. Am. Oil Chem. Soc., 63, 1027-1031 (1986) [Link to non-patent literature 3] S. Shimizu et al., J. Am. Oil Chem. Soc., 66, 237-241 (1989) [Link to non-patent literature 4] S. Shimizu et al., Lipid, 26, 512 (1991) [Link to non-patent literature 5] Sawada, R. et al., Lipids, 34, 633 (1999) [Link to non-patent literature 6] Kushiro, M. et al., J. Nutr. Biochem., 13, 289-295 (2002) As described above, it became known that epistemon has useful properties. Currently, among the methods that are useful for obtaining compositions enriched epistemical that contain epistemic in concentrations of more than 50 wt.%, the known method of its isolation from epistemologija mixtures, for example, column chromatography. About the however, these methods require complex manufacturing operations, and, moreover, they provide only small amounts of the composition at the same time and they are characterized by low efficiency. There is therefore a need to provide a method of obtaining and devices that are more convenient and are great output. The object of the present invention is a method and apparatus that provide the transformation of stamina in epistemon by epimerization and then recrystallization of sesamin and epistemologica mixture, by means of which possible easy to obtain and with high output composition, which contains epistemon, the share of which in relation to the total weight of stamina and epistemon is more than 50 wt.%, preferably 60 wt.% or more, more preferably 70 wt.% and more. As a result of intensive studies directed towards achieving the above object, the present invention has found that sesamin and epistemic have different solubilities in certain specific oils or fats. Using this difference in solubilities, the authors of the present invention investigated the way recrystallization in certain oils or fats and found that it is possible allocation of epistemon from a mixture of sesamin and epistemon with similar structures. Thus, the authors present izaberete the Oia has developed a way, including the stage of dissolution of the mixture containing sesamin and epistemic (which hereinafter the description will be referred to as a mixture of sesamin/epistemic), when heated in oil or fat and then recrystallization from a solution so that crystallization of epistemon took place selectively, and which is convenient and high yield it is possible for the composition, the content of epistemon in which more than 50 wt.%, preferably 60 wt.% or more, more preferably 70 wt.% and more. It provides an implementation of the present invention. The authors present invention also found that we can use the method of epimerization of stamina treatment of acid catalyst for the industrial preparation of compositions enriched epistemical. Accordingly, the epimerization of processing data acidic catalyst combined with the method of recrystallization in a particular oil or fat, which gave the opportunity to the authors of the present invention to achieve the implementation of the present invention, according to which receive a mixture of sesamin/epistemon with a high content of epistemon. More briefly to develop a method and device used for implementing the method, by which it is possible and with high yield convenient obtaining compositions containing their epistemic in concentrations of more than 50 wt.%, preferably 60 wt.% or more, more preferably 70 wt.% and more, the authors of the present invention has adopted the following approach (1) and (2). It provides an implementation of the present invention. (1) processing stage acid catalyst stamina or compositions containing sesamin (including a mixture of sesamin/epistemic)for the epimerization of stamina and phase selective crystallization of epistemon obtained from a mixture containing as sesamin and epistemic (which hereinafter in the description referred to as a mixture of sesamin/epistemic), by recrystallization combined to obtain a composition, which contains epistemic in high concentrations. (2) a Mixture of sesamin/epistemic used as a raw material that does not conduct the processing of an acid catalyst, and just spend the recrystallization in oil or fat to obtain a mixture of sesamin/epistemic containing epistemic concentration of greater than 50 wt.%. A mixture of sesamin/epistemon, which is also used as raw materials in this way can be obtained by epimerization of stamina treatment of acid catalyst; the appropriate mix of sesamin/epistemic also incorporate other ways, such as appropriate refining and extraction. In addition, the authors present invention has developed a device that is with a block isomerization, where is the epimerization of stamina treatment of acid catalyst either directly or stamina, part of staminodial composition; block crystallization, in which the recrystallization mixture of sesamin/epistemon with the use of oil or grease and line the fluid connecting the isomerization unit and the unit of crystallization; more specifically, the authors present invention has developed a device comprising a reactor (mixer) for mixing siseministeerium.ee oil or fat with an acid catalyst for the reaction of isomerization, a mold for carrying out recrystallization and piping for feeding the reaction solution from the reactor tank for crystallization, if necessary, the pipe for supplying liquid equipped with a filtering device. The authors of the present invention have shown that with the use of devices according to the invention of staminodial oil or fat is convenient and possible to obtain a mixture of sesamin/epistemon with high output that contains epistemic in high concentrations. According to the present invention it is possible convenient and high yield of the implementation of the industrial production of compositions containing epistemic in concentrations of more than 50 wt.%, using as raw material stamina or staminodeus composers who s. Brief description of drawings Figure 1 is a given scheme, reflecting the device according to the present invention, to obtain compositions that contain epistemic in high concentrations. Figure 2 - external view of the device according to the present invention to obtain compositions that contain epistemic in high concentrations. The symbols: 1 - device for production; 2 - the isomerization unit; 3 - block recrystallization; 4 - filtering device; 51, 52 - liquid line. The method of receiving according to the present invention begins with the epimerization of stamina or staminodial composition, so that at least part of stamina undergoes epimerization, thereby obtaining a mixture containing as sesamin and epistemic. Sesamin or siseministeerium.ee composition which is a raw material, can be isolated from sesame seeds or extracted from sesame oil by means of known methods. Usually carry out the following procedure. First extract, the main component of which is staminodial composition intended for use in the present invention, is obtained from sesame oil. At the end of this hold phase extraction and preconcentration using a variety of organic solvents, which are almost the e mixed with sesame oil and which have the ability to extract and dissolve siseministeerium.ee composition. Examples of such organic solvents include acetone, methyl ethyl ketone, diethyl ketone, methanol, ethanol, etc. Alternative extract, the main component of which is sesamin used in the present invention, can be obtained from sesame oil. At the end of this stage sesame oil is uniformly mixed with any solvent, referred to earlier, and then the mixture was kept at low temperature; then carry out the separation of the phases by conventional means, such as centrifugation, and the solvent is evaporated from the fractions containing the solvent. More specifically sesame oil is dissolved in 2 to 10 volumes, preferably 6-8 volumes of acetone, and the solution was incubated overnight at the appropriate temperature, which depends on the type of organic solvent; temperature can be below freezing, usually -10°C or below, preferably -20°C. or below, Pets approximately -80°C. In the oil component is deposited, and the organic component is distilled off from the filtrate obtained by filtration, and then the extract is that as the main component contains sesamin. Alternative sesame oil is mixed with hot methanol or ethanol; the mixture is then incubated at room temperature and the solvent is evaporated from f the shares, containing the solvent. Specifically sesame oil mixed with 2 to 10 volumes, preferably 5-7 volumes of hot methanol (at 50°C and above) or hot ethanol (at 50°C and above) and the extraction was carried out with vigorous stirring. Following this, the mixture is either kept at room temperature, or carry out the separation of phases in the usual way, such as centrifugation, and the solvent is distilled off from the fractions containing the solvent, resulting in the extract, which as the main component contains sesamin. If necessary, may conduct extraction with the use of gas in the supercritical state. From these extracts may receive staminodial composition used in the present invention as a raw material, processing it according to a conventional method such as column chromatography, high performance liquid chromatography, recrystallization, distillation, liquid-liquid countercurrent distribution chromatography, etc. to highlight the desired mixture. Data selection methods are described more specifically. The extracts mentioned previously, is subjected to high performance liquid chromatography on obremenitve columns (ODS) using methanol/water (60:40) as eluent; after removal of the solvent the obtained crystal is s is subjected to recrystallization from ethanol to obtain stamina or staminodial composition, which can be used in the present invention. Sesame oil designed for use in the present invention, can be a refined product or it may be crude product obtained at any stage of the production of sesame oil before bleaching. If desired, sesame oil, you can substitute sesame seeds or sesame oil cake (sesame seeds from which the oil has been pressed to its residual content of 8-10%). In this case, sesame seeds or sesame oil cake can be ground, if necessary with subsequent extraction in the usual way using any solvent, for example one of the solvents mentioned above in relation to the extraction of sesame oil. After separation of the substances remaining after extraction, the solvent is removed from the liquid extract by evaporation or a similar way to obtain the extract. From the thus obtained extract of sesame seeds, sesame extract meal or raw materials of sesame oil using a similar method can be obtained sesamin or siseministeerium.ee composition. Note that sesamin obtained inAsiasari Radixwe compare productivity with sesamin, derived from sesame seeds, sesame oil cake or sesame oil, and the data of the optically active forms may also have been the t to be used in the present invention. In addition mixtures, which can be used as raw material in the present invention is obtained from by-products of the production of sesame oil. Note that the selection of stamina and staminodial compositions used in the present invention, and the method of extraction is not limited to the above. In addition, siseministeerium.ee composition used in the present invention is not limited to the composition derived from sesame oil, sesame meal and sesame seeds, you can use all natural products that contain the above-mentioned mixture of sesamin, according to the present invention. Examples of natural products include theAcanthopoanacis Cortex,the treepaulownia,the bark ofginkgo, Piper retrofractum, Asiasari Radixetc. According to the method of the present invention for producing compositions enriched in epistemical, sesamin or staminodial composition was prepared in the manner described above, by processing for carrying out the epimerization so that at least part of stamina undergoes epimerization of obtaining a mixture containing as sesamin and epistemic. The authors of the present invention have investigated the mechanism of epimerization and found that protonation of stamina, having a structure represented by formula I [Formula ]
causes reactions to the disclosure of the cycle, and is formed isomer of epistemon. Therefore, the epimerization, which occurs in the production method according to the present invention is not limited to a specific method, provided that should proceed the reaction disclosure cycle stamina, thus leading to the formation of epistemon, and example of this is the treatment of acid catalyst, thermal treatment in the presence of inorganic acid and the like. Among these methods is the treatment of acid catalyst is preferred from the viewpoint of the efficiency of epimerization (speed conversion with obtaining epistemon) and ease of implementation. The acid catalysts used for treatment of the acid catalyst include inorganic and organic acid Bronsted, such as sulfuric acid, hydrochloric acid, phosphoric acid and boric acid, a Lewis acid such as aluminum chloride, iron chloride, tin chloride and titanium chloride, montmorillonite, such as acid clay and activated clay, and solid catalysts, typical representatives of which are the catalysts of type zeolites and aluminosilicates, and they can be used either individually or in combination of two or more types. Considering the efficiency of the interaction is the major, subsequent processing and other factors, the use of activated clay is preferred. In this regard, the authors of the present invention have found that if 5% aqueous suspension of acid clay has a pH of 5 or higher, the pH is reduced to a lower value by adding a strong acid like hydrochloric acid to the reaction solution during the reaction (pH preferable to 5% water suspension of 3.7 or less), so that the efficiency of epimerization was as high as when using activated clay. Therefore, it is possible the successful use of acidic clay, the pH is reduced by adding acid. Here we note that if refined sesame oil is used to get the same stamina or staminodial composition, epimerization, which occurs spontaneously in the way of cleaning, will help provide a mixture of sesamin/epistemon. In this case, the stage of epimerization according to the present invention may be omitted; however, the authors of the present invention have found that even if the mixture of sesamin/epistemic used as a source of raw materials, the concentration of epistemon in crystals can be increased by treatment with acid catalyst (activated clay). The reason that the best result is in the processing of an acid catalyst, unknown, but it is preferable to use an acid catalyst even in a mixture of sesamin/epistemon. Thus, the feedstock used for epimerization in accordance with the present invention, may represent sesamin, the cleaning of which have been carried out to achieve the degree of purity of almost 100%, or it may be a mixture of sesamin/epistemon. In the case of a mixture of sesamin/epistemon can use a mixture in which the weight ratio of stamina and epistemon can mainly be from about 99.9:0.1 to 40:60. Sesamin and/or epistemic can also be obtained synthetically. For example, it is known that they can be synthesized according to the method Beroza et al. [J. Am. Chem. Soc. 78, 1242 (1956)], the method Takano et al. [J. Chem. Soc. Chem. Commun. R. 189 (1988)] or the method Suginome et al. [J. Org. Chem. 60, p. 3052 (1955)]. Here again can be omitted above the stage of epimerization when receiving a mixture of sesamin/epistemon. According to the method according to the present invention sesamin or staminodial composition including a mixture of sesamin/epistemic) dissolved either before or after the epimerization in oil or fat when heated to obtain a solution, and the solution is subjected to recrystallization, resulting in possible to obtain a composition containing epistemic in high concentrations. Therefore, the oil or fat in which is dissolved sesamin or sesame is encodergasm composition including a mixture of sesamin/epistemic) according to the present invention, preferably is such that differs in its ability to dissolve sesamin and epistemon, so easy enough to implement their separation by recrystallization. Specific examples of the oil or fat, which can be used include TEXDOC (triglyceride of fatty acids with an average carbon chain length), diacyl glycerol, sesame oil, salad, olive oil, soybean oil, rapeseed oil, corn oil, germ oil, rice and sunflower oil. Specifically, TEXDOC (triglyceride of fatty acids with an average carbon chain length) are preferred for use. Below are the solubility of stamina and epistemon in TEXDOC. [Expression 1]
For convenience, oils and fats, which can be used in the present invention include free fatty acids, such as octanoic acid, and esters of fatty acids, such as octylated. The present invention is distinguished by recrystallization staminodial composition of the oil or fat. If the raw material is of sesamin or stamina Rasa composition with a low content of epistemon, preferred is the epimerization of stamina before recrystallization and then recrystallization of epistemon, subjected to epimerization. Using recrystallization from oils and fats was not known up to the present time, but it is assumed that the viscosity of oils and fats have no effect on the recrystallization step (crystallization) (see example 3), and therefore, as noted above, oil or grease intended for use in the present invention, are preferably chosen from oils and fats, which are distinguished by their ability to dissolve sesamin and epistemon, and they, in particular, is not limited to such property as viscosity. Sesamin or staminodial composition including a mixture of sesamin/epistemic) dissolved in the above-mentioned oils or fats, and the way their dissolution is not limited to any particular method. Depending on the concentration of sesamin or staminodial composition including a mixture of sesamin/epistemic) and the type of oil or fat, they are dissolved by heating generally at 60-160°C., preferably at 80 to 140°C and maintained at this temperature for 5-30 minutes. In the production method of the present invention of sesamin or staminodial composition including a mixture of sesamin/epistemic) is dissolved by heating, and then, when the need is and the solution is treated with acid catalyst (epimerization) and the resulting product epimerization is subjected to recrystallization to separate composition, which contains epistemic concentration of greater than 50 wt.%. Despite the fact that on the way recrystallization in oil and fat affect the concentration of dissolved substances (epistemic) in oil or fat during recrystallization, the presence or absence of seed crystals, the cooling rate and so on, it is not limited to a particular method and may be carried out in the same way as conventional recrystallization, which uses water and organic solvents. In particular, the solution in the oil, which is obtained by treatment of the acid catalyst and which contains a mixture of sesamin/epistemon (approximately 1:1) at a concentration of about 2-50%, placed in a crystallizer and cooled slowly, with optional stirring in the presence of about 0.1-20% seed crystal at a temperature maintaining a supersaturated state, preferably in the range of 5-90°C, resulting in a suspension of crystals, which contains epistemic concentration of greater than 50 wt.%. From the suspension obtained in this way, you can select the desired song, enriched epistemical, in the form of crystals at the stage filtration in the presence of obavljenog ethyl alcohol or similar solvents, removal of solvent and drying. The filtrate obtained when the selection contains the remainder of stamina, which was not subjected to recrystallization (sesamin in raw materials or designed for the epimerization of sesamin), if necessary, to this filtrate can be added to a fresh portion of the suspension stamina, and the obtained product with a high concentration of sesamin can be returned as a raw material in the production of the present invention. Sesamin is expensive, but from an economic point of view it is preferable for the production of fresh epistemon by recycling stamina. According to the present invention proposes a method of obtaining compositions enriched epistemical, which includes the stage of dissolution of stamina or staminodial compositions in oil or fat when heated, if desired, processing the acid catalyst to obtain a solution in oil or fat and selective crystallization of epistemon obtained by epimerization of epistemon, by recrystallization. Hereinafter described in detail with reference to the drawings, the principle of the device of the present invention to obtain a composition containing epistemic in high concentrations. 1 shows a diagram of the device for epistemologica composition, as a whole convoy is asenovo 1, and figure 2 shows its experimental implementation. The device 1 for producing epistemologica composition includes the isomerization unit 2 and unit crystallization 3, in which recrystallization is carried out. The isomerization unit 2 includes a mixer 21, which siseministeerium.ee oil or fat, which includes staminodial composition dissolved in the oil or fat is mixed with the acid catalyst. The mixer 21 is a tank for the reaction in which sesamin lead in the interaction with the acidic catalyst for isomerization reactions; to ensure that the isomerization reaction took place, the mixer 21 is preferably equipped with a device for heating (not shown), which provides, if required, heated to 60-160°C., preferably to 80 to 140°C and maintaining this temperature for 5-60 minutes, preferably 10-30 minutes. You can use the usual devices for heating, such as electric heater and device for use of superheated steam. In addition, the device for mixing 22 if necessary, can be installed mainly in the center of the mixer so that the temperature of the reaction solution was the same, and/or to accelerate the reaction by accelerating contact sesame is containing oil or fat and an acid catalyst. Device for mixing 22 includes a mixer 221, consisting of a shaft a and blades 221b, with the control unit 222 located above the mixer 221. Sesame oil can be an oil or fat, which contain a sufficiently large number of stamina intended for crystallization in block crystallization, and his example is sesame oil obtained by extraction with supercritical solvents; however, to confirm the effective deposition of epistemon it is preferable to use oil or fat is mixed with sesamin or staminodial composition, which is then dissolved in the oil or fat when heated. Phase dissolution during heating can be carried out in the mixer 21 during the mixing stamina with acid catalyst. In this case, the mixer 21 is preferably equipped with an input opening through which serves powder, and a funnel (not shown), from which it is served. In the isomerization unit 2, the reaction solution containing epistemic, subjected to epimerization, taken from the mixer 21 via the outlet port 23 and serves to block the crystallization of 3 for the fluid lines (51, 52), between which there is a filtering device 4. For opening and closing the outlet 23 is a valve ON/OFF (not shown), which remains closed with the exception of the epimerization reaction in the mixer 21 and opens at the end of the interaction, providing a displacement reaction solution in a certain direction. The reaction solution discharged from the mixer 21 through the fluid (reaction solution is supplied by pipeline 51) for filing a filtering device 4. The filtering device may be of any type, with which you can remove the acid catalyst, the specific example is a membrane filter, but you must choose this, which operation is possible at temperatures (high temperature) solution of the reaction. For quick filter filtering device 4 is preferably equipped with a device for supplying under pressure or vacuum system. In addition, if the temperature of the reaction solution drops, crystals stamina or epistemon potentially can settle, so it is preferable to equip the filtering device 4 device for heating. Among the devices for heating includes a device for maintaining a high temperature, which prevents the falling of the temperature of the reaction solution. An example of a device for maintaining a high temperature may be an insulating material, which covers the pipeline to supply the reaction solution 51 and the filtering device 4. The filtrate is separated by a filtering device 4, passes through drobopro the remote control 52 for conveying filtrate, intended for submission to the vessel for crystallization 31 in block crystallization 3. The principle of operation of the device according to the present invention for the production of epistemologica composition based on the difference in solubilities of stamina and epistemon and recrystallization in oil or fat for the Department of epistemon from a mixture of sesamin and epistemon with similar structures. Specifically epistemiology hot reaction solution is cooled in the vessel for crystallization 31 to a temperature at which the solubility lower than that of the solubility at saturation, after which epistemon precipitates from the supersaturated solution. So the tank for crystallization 31 preferably equipped with a cooling device (not shown). The principle of operation of the device for cooling can be based on cooling by heat exchange with refrigerant or cooling by evaporation of part of the solvent under reduced pressure; however, if the cooling rate is too high, the density of the deposited crystals becomes so low that they have the potential to enable a large number of solvent oil or fat; however, in the case of cooling by the cooling medium is not recommended to use ice and the like as a cooling substance, but the preferred one is to use water or air at a temperature of from about zero to about ordinary temperatures, preferably up to about 5 to 20°C. the Vessel for crystallization 31 preferably equipped with a device for mixing 32 mainly in the centre to ensure the same temperature of the filtrate in the tank. Device for mixing 32 includes a mixer 321, consisting of the shaft 321a and blade 321b, the control unit 322 located above a mixer 321. At the time when the filtrate in the tank for crystallization 31 is cooled to some extent, it is preferable to add the seed crystals for exercising crystallization, at the end as the outlet of the vessel for crystallization 31 use the hole through which filed the seed crystals. If the mixer 21 and the vessel for crystallization 31 provided with a viewing window, this allows you to ensure that sesamin and epistemic dissolve when heated, which was carried out processing of clay and that was recrystallized (precipitation of crystals during crystallization). The suspension containing the precipitated crystals are then removed from the vessel for crystallization 31 via the outlet port 33, thereby obtaining the desired epistemic. In order to emphasize crystals from a suspension means for the selection of crystals, such as a vacuum system or otherwise, the filtering unit or the unit price is trippynova, can be installed on the line either continuous or periodic device according to the present invention for the production of enriched epistemologica composition.In addition you can use the device through which the filtrate from which you have removed the desired crystals, again fed into the mixer 21 for reuse of the solvent oil or fat. Further, optionally, in order to increase the purity of epistemon crystals washed with additional organic solvent, such as ethyl alcohol, then filtered and, if necessary, they can be dried either continuously or periodically according to the present invention. [Example] In the description of the present invention will be described more specifically with reference to the following examples which do not limit the present invention. [Test cases] Epimerization of stamina (Test example 1) 3-necked flask with a capacity of 100 ml of the solvent were weighed 20 g of toluene; then the flask was placed 4.0 g of a mixture of sesamin/epistemic (the ratio of the component of sesamin/epitamy of 99.1/0.9) and was heated on an oil bath to 110°C with stirring until the mixture is fully dissolved. To the solution was added 0.6 g of activated clay (product of MIZUSAWA INDUSTRIAL CHEMICALS, LTD., the trademark “GALLEON EARTH V2R) as kislotno the catalyst and the mixture was stirred at 110°C. Then the reaction time was monitored by HPLC analysis under the conditions below; after 5 minutes it was found that the output of epistemon is 48%. (HPLC) Column: Inertsil ODS-3 (GL-SCIENCE) of 4.6·150 mm; The column temperature: 25°C; Mobile phase: methyl alcohol/water = 7:3; Flow rate: 1 ml/min; Detector: UV 290 nm. (Test example 2) 3-necked flask with a capacity of 100 ml of the solvent were weighed 20 g of benzene; then the flask was placed 4.0 g of a mixture of sesamin/epistemic (the ratio of the component of sesamin/epitamy of 99.1/0.9) and was heated on an oil bath to 80°C with stirring until the mixture is fully dissolved. To the solution was added 0.6 g of activated clay (product of MIZUSAWA INDUSTRIAL CHEMICALS, LTD., the trademark “GALLEON EARTH V2R) as the acid catalyst and the mixture was stirred at 110°C. Then the reaction time was monitored by HPLC analysis under the same conditions as in test example 1; in an hour it was found that the epimerization took place with the release of approximately 49%. (Test example 3) 3-necked flask with a capacity of 100 ml of the solvent were weighed 20 g of toluene; then the flask was placed 4.0 g of a mixture of sesamin/epistemic (the ratio of the component of sesamin/epitamy of 99.1/0.9) and was heated on an oil bath to 110°C with stirring until the mixture is completely not what actuaries. To the solution as an acid catalyst was added 0,78 g D camphor-10-sulfonic acid (product of nacalai tesque), and the mixture was stirred at 110°C. Then the reaction time was monitored using HPLC under the same conditions as in test example 1; the education of epistemon occurred gradually and after 20 hours it was found that the output of epistemon was approximately 48%. When the number of added D-camphor-10-sulfonic acid to 1.30 g after 2 hours the output of epistemon was approximately 43%; after 18 hours of reaction during the night the yield increased to about 49%, which provided the ratio of epistemic/sesamin when receiving approximately 1:1. (Test example 4) In a test tube with a removable lid with a capacity of 70 ml of the solvent were weighed ethanol (5.0 ml); then the tube was placed 96 mg of a mixture of sesamin-epistemic (the ratio of the component of sesamin/epistemic 99,1/0,9), closed with a lid and heated in an oil bath to 83°C with stirring until the mixture is fully dissolved. To the solution was added as an acid catalyst 1.2 ml of hydrochloric acid (product of nacalai tesque, containing 35% HCl) and then closing the lid, the mixture was stirred at 110°C. Then the reaction time was monitored using HPLC under the same conditions as in test example 1; cher is C 2 hours was found, the output stamina is approximately 49%. (Test example 5) In pear-shaped flask with a capacity of 20 ml were placed in 5.0 ml of telengard and 96 mg of a mixture of sesamin/epistemic (the ratio of the component of sesamin/epistemic 99,1:0,9); then at a lower temperature -83°C. the mixture was stirred for 10 minutes while bubbling nitrogen. To the solution as an acid catalyst was added 72 mg of aluminium chloride (a product of Sigma Aldrich). Then the reaction time was monitored using HPLC under the same conditions as in test example 1; after 30 minutes it was found that the output is approximately 21%. [Example 1] In pear-shaped flask with a capacity of 50 ml was weighed 20 g of oil or fat; then the flask was placed 2.8 g of a mixture of sesamin-epistemic (the ratio of the component of sesamin/epitamy of 99.1:0.9) and was heated on an oil bath to 120°C with stirring until the mixture is fully dissolved. To the solution was added 0.4 g of activated clay (product of MIZUSAWA INDUSTRIAL CHEMICALS, LTD., the trademark “GALLEON EARTH V2R) as the acid catalyst; followed by treatment for 30 minutes at 120°With old clay was removed by filtration. Part of the filtrate was collected as a sample for HPLC (sample 1). The remaining liquid was slowly cooled in air at 20°C; when the liquid temperature reached 60°C, was added 2.8 mg seed Crist is low 100% of epistemon and crystallization was carried out for 30 minutes in air at 20°C. The liquid containing precipitated crystals were subjected to separation into liquid and solid phase by filtration under vacuum and the solvent remaining in the crystalline mixture was washed with 99.5% ethanol. Selected crystalline mixture (sample 2) was analyzed by HPLC. Analysis of the composition of sesamin/epistemic was performed using HPLC under the conditions below. The results of the analysis are shown in table 1 (in which the purity of epistemon concentration (wt.%) epistemon in crystalline mixture). (HPLC) Column: Inertsil ODS-3 (GL-SCIENCE) of 4.6·150 mm; The column temperature: 40°C; Mobile phase: methyl alcohol/water = 7:3; Flow rate: 1 ml/min; Detector: UV 290 nm. The viscosity measurement was carried out on viscosimetry Model VT-04 (product RION Co., Ltd.), rotor No. 3, and the temperature of the liquid oil or fat was brought to 20°C. the Speed of rotation was at 62.5 rpm and readings were off 10 seconds after the start of deceleration of the rotor for measuring the viscosity of the test oil or fat.
As is clear from table 1, it is possible to obtain compositions with 65 wt.% and more epistemon when used as a fat or oil TEXDOC, diacyl glycerol, olive oil, sesame oil for salad, soybean oil, germ oil, rice, rapeseed oil, corn oil, sunflower oil, octanoic acid and octyl acetate. Specifically, it was found that it is possible to obtain compositions with 80 wt.% and more epistemon when using diacyl glycerol, olive oil, soybean oil, germ oil, rice, rapeseed oil and sunflower oil, and that the composition of 90 wt.% and more epistemon can be obtained by using TEXDOC, octanoic acid and octyl acetate. [Example 2] In pear-shaped number of the e capacity of 50 ml was weighed 20 g of oil or fat; then the flask was placed 4.0 g of a mixture of sesamin-epistemic (the ratio of the component of sesamin/epistemic 55/45) and was heated on an oil bath to 120°C with stirring until the mixture is fully dissolved. To the solution was added 0,57 g of activated clay (product of MIZUSAWA INDUSTRIAL CHEMICALS, LTD., the trademark “GALLEON EARTH V2R) as the acid catalyst; followed by treatment for 30 minutes at 120°With old clay was removed by filtration. Part of the filtrate was collected as a sample for HPLC analysis (sample 1). The remaining liquid was slowly cooled in air at 20°C; when the liquid temperature reached 60°C, was added 4.0 mg seed crystals 100% of epistemon and crystallization was carried out for 30 minutes in air at 20°C. the Liquid containing precipitated crystals were subjected to separation into liquid and solid phase by filtration under vacuum and the solvent remaining in the reaction mixture, washed with 99.5% ethanol. Restored thus crystalline mixture was observed (sample 2). Similarly, in a pear-shaped flask with a capacity of 50 ml was weighed 20 g of oil or fat (TEXDOC; ACTOR M-1 manufactured by RIKEN VITAMIN CO., LTD.); then the flask was placed 4.0 g of a mixture of sesamin-epistemic (in the compositional ratio of sesamin/epistemic 55/45) and was heated on an oil bath to 120°C with stirring until the mixture is completely not RA what was happening; part of the solution was collected as a sample for HPLC analysis (sample 3). The remaining liquid was cooled slowly in air at 20°C; when the liquid temperature reached 60°C, was added 4.0 mg seed crystals 100% of epistemon and crystallization was carried out for 30 minutes in air at 20°C. the Liquid containing precipitated crystals were subjected to separation into liquid and solid phase by filtration under vacuum and the solvent remaining in the reaction mixture, washed with 99.5% ethanol. Restored so the mixture was analyzed by HPLC (sample 4) to analyze the composition of sesamin/epistemon. The HPLC conditions are the same as in example 1. The results are shown in table 2.
As is clear from table 2, the processing of clay promotes the elicerio content of epistemon end of the obtained composition. [Example 3] In pear-shaped flask with a capacity of 50 ml was weighed 20 g of oil or fat (TEXDOC; ACTOR M-1 manufactured by RIKEN VITAMIN CO., LTD.); then the flask was placed 2.8 g of a mixture of sesamin-epistemic (the ratio of the component of sesamin/epitamy of 99.1:0.9) and was heated on an oil bath to 120°C with stirring until the mixture is fully dissolved. To the solution was added 0.4 g of activated clay (each sample of which is produced by MIZUSAWA INDUSTRIAL CHEMICALS, LTD.) as the acid catalyst with subsequent treatment for 30 minutes at 120°With old clay was removed by filtration. Part of the filtrate was collected as a sample for HPLC analysis. Performed HPLC for the thus obtained sample for analysis of the composition of sesamin/epistemon in the conditions below. The results of the analysis are shown in table 3. (HPLC) Column: Inertsil ODS-3 (GL-SCIENCE) of 4.6·150 mm; The column temperature: 40°C; Mobile phase: methyl alcohol/water = 7:3; Flow rate: 1 ml/min; Detector: UV 290 nm.
[Example 4] As shown in example 3, the presence of an acidic clay did not provide comparable isomerization reaction, therefore, was tested in order to see, did the results of adding a reaction solution of a strong acid, comparable with those obtained for the activated clay (pH of the suspension is measured using a strip of pH test paper was approximately 1). In pear-shaped flask with a capacity of 50 ml was weighed 16 ml TEXDOC (ACTOR M-1 manufactured by RIKEN VITAMIN CO., LTD.) and 4 ml of 5 N HCl; later in the flask were placed 2.8 g of a mixture of sesamin-epistemic (the ratio of the component of sesamin/epitamy of 99.1:0.9) and then set the reflux condenser, the flask was heated on an oil bath to 120°C with stirring until the mixture is fully dissolved. To the solution was added 0.4 g of acid clay (MIZUKA ACE #400 produced by MIZUSAWA INDUSTRIAL CHEMICALS, LTD.) and the reaction was carried out for 30 min is t at 120°C. After completion of the reaction, an elaborate clay was removed by filtration, and the part of the filtrate was collected as a sample for HPLC analysis. Analysis conditions were the same as in example 1. In the HPLC analysis revealed that the ratio of sesamin/epistemic was 53,7/41,0, indicating that the isomerization reaction was comparable to that obtained with activated clay. [Example 5] Epistemic was obtained from siseministeerium.ee oil or fat with the use of the device for the production of enriched epistemologija compositions, which marked 1 in figure 1. Specifically, 2500 g TEXDOC (ACTOR M-1 manufactured by RIKEN VITAMIN CO., LTD.) weighed in a mixing tank 21, in which were placed 360 g of a mixture of sesamin-epistemic (in the compositional ratio of sesamin/epitamy of 99.1:0.9) and was heated on an oil bath to 120°C with stirring until the mixture is fully dissolved with the formation of staminodial solution of the oil or fat. In the mixing tank 21, now containing a solution of oil or fat, added 54 g of acid catalyst (activated clay, produced by MIZUSAWA INDUSRIAL CHEMICALS co., LTD. under the trademark “GALLEON EARTH V2R”) followed by treatment for 30 minutes at 120°C, the liquid is subjected to processing, under pressure, was passed through a membrane filter (filtering device 4) for simultaneous removal the Oia waste clay. The resulting liquid (approximately 100°C) was sent to the vessel for crystallization 31 in block crystallization 3 and slowly cooled with cold water. After about 15 minutes, when the liquid temperature reached 60°C, made of 720 mg of epistemon (99.9% purity) as the seed crystals and the crystallization was carried out for 90 minutes with slow stirring. The resulting suspension (approximately 25-30°C) was extracted via the outlet port 33. Then spent the separation of the liquid and solid phase by filtration under vacuum and the crystals were washed with ethanol to obtain the desired crystals in the number 90,8 g (yield 26.0 per cent). Thus obtained sample for analysis of the composition of sesamin/epistemic was subjected to HPLC under the conditions below; purity of epistemon stood at 95.6%. (HPLC) Column: Inertsil ODS-3 (GL-SCIENCE) of 4.6·150 mm; The column temperature: 40°C; Mobile phase: methyl alcohol/water = 7:3; Flow rate: 1 ml/min; Detector: UV 290 nm. Application in industry According to the present invention as a source of raw materials used by sesamin 100% purity or siseministeerium.ee composition, for example, a mixture which contains as sesamin and epistemon, result and high yield convenient obtaining compositions that contain EPI is etamin concentration of greater than 50 wt.%. 1. The production method of the composition, enriched with epistemical containing epistemic concentration of greater than 50 wt.%, including the stage of implementation of the epimerization of stamina or staminodial composition so that at least part of stamina becomes epistemon; and crystallization of epistemon by recrystallization. 2. The method according to claim 1, in which a composition enriched in epistemical represents the precipitated crystals and contains epistemon at a concentration of 60 wt.% and more. 3. The method according to claim 1, in which a composition enriched in epistemical includes 70 wt.% or more epistemon. 4. The method according to claim 2, in which a composition enriched in epistemical includes 70 wt.% or more epistemon. 5. The method according to any one of claims 1 to 4, which, in addition, includes a step of dissolving stamina or staminodial compositions in oil or fat when heated either before or after epimerization, obtaining, thus, of solution. 6. The method according to claim 5, in which the oil or fat is selected as one of TEXDOC (triglyceride of fatty acids with an average carbon chain length), diacylglycerol, salad sesame oil, olive oil, soybean oil, rapeseed oil, corn oil, germ oil, rice and sunflower oil. 7. The method according to claim 5, in which the oil or fat is TEXTU the (triglyceride of fatty acids with an average carbon chain length). 8. The method according to any one of claims 1 to 4, 6 and 7 in which the epimerization represents the processing of an acid catalyst. 9. The method according to claim 8, in which the processing of an acid catalyst consists in bringing into contact with activated clay or acid clay. 10. The method according to claim 9, in which an activated clay or acid clay is such a pH of 5% aqueous suspension was reduced to 3.7 or less. 11. The method according to PP or 10, in which an activated clay or acid clay has a specific surface area of 150-350 m2/year 12. The method according to any one of claims 1 to 4, 6, 7, 9 and 10, which, in addition, includes a step of extracting crystals that were deposited by recrystallization, filtration. 13. The method according to any one of claims 1 to 4, 6, 7, 9 and 10, in which the leachate generated at the stage filtration, is returned to the step of obtaining a solution. 14. The method according to any one of claims 1 to 4, 6, 7, 9 and 10, in which the feedstock is either 100% of sesamin, or a mixture of sesamin and epistemon with weight ratio stamina and epistemon of 99.9:0.1 to 40:60. 15. Device for the production of stamina, subjected to epimerization, including the isomerization unit, comprising a mixing tank for mixing oil or fat containing sesamin or staminodial composition with an acid catalyst for the reaction block of crystallization, including a reservoir for crystallization to conduct recrystallization, and the supply line of the fluid connecting the mixing tank with the tank for crystallization. 16. Device for the production of stamina, subjected to epimerization, § 15, in which a liquid channel is equipped with a filtering device. 17. Device for the production of stamina, subjected to epimerization, in P16, in which the supply line of the liquid consists of a pipeline for feeding the reaction solution from the mixer to the filtering device and the pipeline to move the filtrate from the filter unit into the vessel for crystallization. 18. Device for the production of stamina, subjected to epimerization, p-17, in which the isomerization unit includes a device for heating the mixer. 19. Device for the production of stamina, subjected to epimerization, PP and 17, in which the filtering device includes a heating device. 20. Device for the production of stamina, subjected to epimerization, PP and 17, in which the filtering device includes a device that provides flow under pressure. 21. Device for the production of stamina, subjected to epimerization, PP and 17, in which the vessel for crystallization includes a cooling device.
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