A method of processing a neutral substances
(57) Abstract:The invention relates to methods for processing of neutral substances secreted from low-grade hardwood sulfate soap, and can be used in the pulp and paper and timber industry for cleaning of sulfate soap from cooking a mixture of different species of wood including birch. In the processing of low-quality sulfate soap the traditional way to improve the quality obtained from tall oil, pre-extracted neutral compounds containing biologically active compounds: betulin, sterols, polyprenols, squalene. Known methods of processing the extracted neutral substances highlight only one or two of the listed biological active compounds. The proposed method for the processing of neutral substances sulfate soap allows one process stream to obtain concentrates all of these biologically active compounds: betulin ("sitemeta"), sterols ("cristial"), polyprenols, squalene. The proposed method is based on the use of differences in physico-chemical constants and chemical properties of individual groups and individual H filtering and extraction using selective between immiscible solvents. table 2. The invention relates to chemical and pulp and paper industry, namely the processing of neutral substances secreted from low-grade hardwood sulfate soap.There is a method of processing a neutral substances with the separation of sterols through the formation of complexes with the chloride of the metal 
There is a method of processing a neutral substances, with the separation of sterols from one stripped off an ethyl acetate extract of neutral substances by addition of water 
There is a method of processing a neutral substances with the release of phytosterol extraction with a mixture of hexane, acetone, methanol and water 
There is a method of processing a neutral substances with the release of phytosterol, processing aromatic hydrocarbon, a polar solvent with the addition of water 
The method for extracting sterols from neutral substances from the mixture of solvents: hexane, xylene, ethyl acetate and water 
Known methods of processing of neutral substances emitting sitosterol and the form of the hydrate of a mixture of sterols by treatment with an organic solvent [6, 7]
There is a method of processing a neutral substances emitting sitosterol treatment m the low-quality hardwood sulfate soap, with the release of betulin  beaupreau (polyprenols)  "cytometry" 
However, all these methods are aimed at the separation of neutral substances with floor doctrine as the end product of one or two compounds. Other compounds included in the composition of the neutral substances are not used.The closest in technical essence and the achieved result for the proposed method is a method of processing a neutral substances sulfate soap from cooking a mixture of different species of wood including birch, which consists in extracting neutral substances with ethyl acetate, evaporation of the extract neutral substances to the dry matter content of 10 to 33.3% cooling one stripped off of the extract to a temperature of 18 of the 22oC and crystallized from the cooled solution "cytometry" within 2 9 h 
The disadvantage of this method is its low efficiency, which is caused by the product of cytometry", containing two main biologically active compounds sitosterol and betulin.The objective of the invention increase the efficiency of the method of processing of neutral substances produced from low-grade hardwood sulfate soap, by allocating additional the processing of low-sulfate soap from cooking a mixture of different species of wood, including birch, soap extracted with ethyl acetate in the presence of water, separating the extract from the raffinate is distilled off from the extract of the extractant and produce a neutral substance that is transferred to the hydrocarbon solvent extraction gasoline, petroleum ether, nefras and others), when the content of dry substances in a solution of 1,4 9,0% washed with water or 2 5%-s ' solution of the hydroxide or carbonate of an alkali metal at a ratio of water: the solution is neutral substances equal to 0.5 to 5.0:1.0 for exemption from traces of salts of organic acids and solids, defend 0.25 to 2 h at a temperature of -30 +20oC. the Precipitated crystals betulin or "cytometry" separated by filtration and dried. The product yield is 3 to 15% of the amount of neutral substances passing into a hydrocarbon solvent.The solids content in the solvent should not be less than 1.4 percent as in this case sharply reduced yield of betulin. With the increasing content of dry substances in the solvent than 2% cannot obtain pure betulin, as it begins simultaneously with betulin crystallization of sterols, while receiving the drug cytolethal". When the content of dry substances in solution more than 9% difficult operation full the I water: the solution is neutral substances is not determinative for the separation, but keeping it in the range of 0.5 to 5.0:1.0 to allows you to achieve a complete mixing system and, consequently, better removal of impurities. Increasing the volume of water greater than 5.0: 1.0 is rational due to the increase in equipment and energy consumption for mixing. The introduction of small amounts of alkali or soda to pH 8 9 shifts the equilibrium for organic acids towards the formation of soluble salts in water and therefore increases the efficiency of their Department. Increasing the concentration of alkali (soda) is impractical because at pH 8 9 already almost complete transition of organic acids from the molecular ion in the form.Crystallization of less than 0.25 h decreases the yield of betulin ("cytometry") that with increasing time of crystallization of more than 2 h does not increase.Increasing the crystallization temperature above 20oWith leads to reduction of yield of betulin, lowering the crystallization temperature to -18oC and crystallization time over 0.5 h leads to an increase in deposition simultaneously with betulin sterols, and at temperatures below -18oC also begin to precipitate aliphatic alcohols. Further lowering of the temperature below -30oC economically netsales the dry substances 10 33,3% then cooled to a temperature below 0oC and kept at this temperature for 1 to 3 hours this stands a crystalline product, which could be called the drug "cristial". The output of this product is 5 to 10% of neutral substances."Cristial" the white crystalline product containing 30 to 40% of betulin, 30 to 40% of a sitosterol /carotovora/, 8 12% b-sitosterol and 10 to 20% of aliphatic alcohols from 24 to 28 carbon atoms. The melting interval "Kristiana" 170 220oC.The solids content in the solution during the precipitation of "Kristiana" should not exceed 33.3% of as otherwise impeded the operation of the filter due to the high solution viscosity. When the solids content in the solution is below 10% reduced yield a crystalline precipitate.Increasing the crystallization temperature above 0oC leads to a decrease in the content of higher aliphatic alcohols in "cristyle", which in turn leads to contamination of the concentrate polyprenols and squalene remaining neutral substances aliphatic alcohols, for the removal of which requires an additional operation of crystallization. Division of polyprenols and higher aliphatic alcohols is one of the most difficult tasks. When the crystallization temperature below -18oThe filtrate 11 after selecting "Kristiana" evaporated to trace amounts of solvent. Selected neutral substances extracted aprotic polar solvent.The raffinate after separation of the residue of the extractant is a concentrate containing Sterol, triterpene and aliphatic alcohols with a residual content of hydrocarbons and polyprenols.The selected extract is washed (extracted) hydrocarbon dissolution and after distillation of the solvents get two products. First - viscous dark-colored product, a mixture of polyfunctional oxidized compounds. The second concentrate polyprenols and squalene. Further, if necessary, polyprenols separated from squalene adsorption liquid chromatography and get concentrate polyprenols and concentrate squalene. The output of concentrate polyprenols 22 24% yield of concentrate squalene 3 6% from neutral substances. The data are given in table. 1 and 2.Example 1. 170 g hardwood sulfate soap, with a humidity of 50% is dissolved in 170 ml of water, then add 110 ml of ethylacetate. The whole mixture is stirred until the formation homogenates neutral substances, fending off the ethyl acetate. Get was 12.75 g of neutral substances which dissolve in 637,5 g of gasoline, you get a solution neutral substances solids content in the solution is 2% of the resulting solution was washed with 350 ml of 2% aqueous solution OH defend at a temperature of 20oC for 2 hours fall At the same time the crystals betulin 0,38 g, which is separated from the solution by filtration. From the filtrate distilled 550 g of gasoline, get a solution of neutral substances with a solids content in the solution is 14% which is cooled to -3oC and kept at this temperature for 1 h From the solution falls crystals of sterols, which are separated from the solution by filtration. Obtain 1.3 g of sterols. Then from the filtrate evaporated gasoline, and the remaining neutral substances extracted aprotic polar dissolution, then washed extract (extracted) hydrocarbon solvent is distilled off the solvent and receive (3.77 g) concentrate of polyphenols and squalene. The concentrate of polyphenols and squalene share of liquid adsorption chromatography to concentrate pranolol (3.12 g) and concentrate squalene (0,65). In addition to these products as waste get the raffinate (7.0 g) and concentrate polyfunctional oxidized compound (1.3 g).about alcohol at a temperature of 60oC, then for 15 minutes the resulting solution was extracted with petrol (800 g) at a temperature of 40othen extract the neutral substances are separated from sulfate soap. The extract obtained (700 g) is a solution of neutral substances in gasoline (hydrocarbon solvent) content of dry substances in a solution of 1.4% Solution of neutral substances washed with water (700 g), then prepare the chin at a temperature of +4oC for 0.5 hours, fall at the same time the crystals betulin, which is separated by filtration from the solution of neutral substances. Get the concentrate betulin (0.45 g). The filtrate is evaporated to a solids content in the solution is 20% distilled 656,8 g gasoline), cooled to -5oC and kept at this temperature 0,25 hours From the solution drop crystals sterols, which are separated from the solution by filtration. Obtain 1.35 g of the concentrate of sterols. From the filtrate evaporated gasoline, and the remaining neutral substances extracted aprotic polar solvent, and then hydrocarbon solvent is distilled off the solvent and obtain a concentrate of polyprenols and squalene (2.3 g). Concentrate polyprenol and squalene share in a known manner to concentrate pranolol (2,03 g) and conc). A method of processing a neutral substances containing betulin, sterols, polyprenols and squalene, by extraction with an organic solvent, namely, that of a neutral substance is transferred into the solution of the hydrocarbon solvent, which is washed with 2 5% aqueous-alkaline solution, followed by crystallization and filtration of the solution neutral substances emit concentrate betulin content of dry substances in a solution of 1,4 2,0% then concentrate Sterol content of dry substances in a solution of 3.0 33.3% and a crystallization temperature below 0oAnd from the filtrate after removal of the solvent allocate remaining neutral substance, which is extracted aprotic polar solvent, and then hydrocarbon solvent is distilled off the solvent and produce a concentrate of polyprenols and squalene, which is then separated in a known manner adsorption, liquid chromatography to concentrate polyprenols and concentrate squalene.
an intermediate product in the synthesis of natural phytohormone of epibrassinolide with high growth promoting activity (1-3)
which is an intermediate substance to obtain (22R, 23R)-3- acetoxy-22,23-isopropylidenedioxy-24-metalholic-5 - ene of formula II;
Compound II is a well-known synthetic precursor hormone brassinolide) III, which is found in very low concentrations in some plants and is the most active of the new class of natural hormones - steroids, and therefore can be used in agriculture as a growth promoter, plant /1/
cholesterol (Chs)< / BR>testosterone (TS)which can be used as source reagents for solid-phase synthesis of steroid derivatives of oligonucleotides and their analogues
FIELD: organic chemistry, steroids, medicine, pharmacy.
SUBSTANCE: invention relates to 3-methylene-steroid derivative of the general formula (1):
wherein R1 means hydrogen atom (H), or in common with R3 it forms β-epoxide; or R1 is absent in the presence of 5-10-double bond; R2 means (C1-C5)-alkyl; R3 means βH, βCH3 or in common with R1 it forms β-epoxide; either R3 is absent in the presence of 5-10-double bond; R4 means hydrogen atom, lower alkyl; Y represents [H, H], [OH, H], [OH, (C2-C5)-alkenyl], [OH, (C2-C5)-alkynyl] or (C1-C6)-alkylidene, or =NOR5 wherein R5 means hydrogen atom (H), lower alkyl; dotted lines represent optional double bond. Compound can relate also to its prodrug used for treatment of arthritis and/or autoimmune diseases.
EFFECT: valuable medicinal properties of compounds, improved method for treatment.
38 cl, 1 tbl, 18 ex
FIELD: organic chemistry, medicine, pharmacy.
SUBSTANCE: invention represents new derivatives of 17,20-dihydrofusidic acid of the formula (Ia)
wherein Q1 and Q2 are similar or different and mean -CO-, -CHOH-, -CHRO- wherein R means (C1-C4)-alkyl; Q3 means -CH2-; Y means hydrogen atom (H); A means -O- or -S-; R1 means (C1-C4)-alkyl, (C2-C4)-olefin, (C1-C6)-acyl, (C3-C7)-cycloalkylcarbonyl, benzoyl. These derivatives are used in pharmaceutical compositions for treatment of infectious diseases, in particular, in composition for topical applying for treatment of infectious diseases of skin and eyes.
EFFECT: valuable medicinal properties of compounds.
22 cl, 7 tbl, 41 ex
FIELD: organic chemistry, chemistry of steroids.
SUBSTANCE: invention relates to a new method for synthesis of 6β-formyl-B-norcholestane-3β,5β-diol of the formula (I): by constricting six-membered B-ring of cholesterol. Method involves photooxidation of cholesterol with air oxygen at irradiation by visible light in the presence of porphyrine photosensibilizing agent immobilized on low-molecular fraction of copolymer of tetrafluoroethylene and perfluoro-3,6-dioxo-5-methyl-6-sulfonylfluoride octene-1 in the mass ratio porphyrine photosensibilizing agent : cholesterol = 1:(12-15). As porphyrine photosensibilizing agent 5,10,15,20-tetraphenylporphyrine can be used. Method shows technological simplicity, it doesn't require rigid conditions and provides the high yield of the end product.
EFFECT: improved preparing method.
2 cl, 3 ex
FIELD: medicinal industry, sterols.
SUBSTANCE: invention relates, in particular, to the improved method for producing sterols - lanosterol and cholesterol from wooly fat that can be used in preparing medicinal and cosmetic preparations. Method is carried out by alkaline hydrolysis of raw, extraction of unsaponifiable substances, removal of solvent and successive isolation of lanosterol and cholesterol. Alkaline hydrolysis of raw is carried out with a mixture of ethanol, sodium hydroxide, pyrogallol and water at temperature 70°C for 4 h at stirring in the following ratio of components: raw : ethanol : sodium hydroxide : pyrogallol : water = 100.0:(300.0-350.0):(30.0-35.0):(0.01-0.05):(7.5-12.0), respectively, with the indicated mixture with addition of toluene in the following ratio: raw : ethanol : sodium hydroxide : pyrogallol : toluene : water = 100.0:(220.0-255.0):(30.0-38.0):(0.05-0.12):(100.0-137.0):(2.5-7.0), respectively, and lanosterol is isolated by precipitation from mixture of methylene chloride and ethanol in the ratio = 1:1. Before removal of solvent unsaponifiable substances are extracted at temperature 50°C for 2-3 h at stirring. Invention provides increasing yield of the end product, enhancing qualitative indices and reducing cost of production.
EFFECT: improved producing method.
2 cl, 3 ex
SUBSTANCE: polyaminosteroid branched derivatives of general formula I are described, where R1 is saturated or unsaturated C2-C10alkyl (conjugated or branched) or methyl, R2 is COOH or branched polyamine fragments, R3 is H, OR19, where R19 is H or C1-6acyl, R4 is H, R5 is H, CH3, R6 is H, CH3, R7=R8=R9=H, R10 is H, CH3, R11 is OH,-OSO3, - O-acyl, -(Z)n-(NR-Z)p-N(R)2, Z is linear hydrocarbon diradical, n=0, 1, p=1, R-H, C1-6alkyl, C1-6aminoalkyl, possibly substituted by C1-6alkyl, R12=R13=R15=H, R16 is H, OH, R17 is H, R18 is H, CH3, possible double bond. Compounds possess bactericidal activity and can be used for prevention of bacterial infections.
EFFECT: production of polyaminosteroid derivatives, possessing bactericidal activity which can be used for prevention of bacterial infections.
27 cl, 31 ex, 1 tbl, 2 dwg
SUBSTANCE: claimed invention describes paroxetine cholate or salt of cholic acid derivative and composition, which contains paroxetine and cholic acid or its derivative. Also described is pharmaceutical composition for treatment of depressive states, containing paroxetine salt or composition. Pharmaceutical composition can be part of peroral medication, swallowed without water, on form of disintegrating in mouth paroxetine tablet.
EFFECT: obtaining paroxetine cholate or salt of cholic acid derivative, which can be used in pharmacology.
19 cl, 38 ex, 12 tbl
SUBSTANCE: invention refers to synthesis of biologically active substances, in particular specifically, to improved method of producing 2,3-monoacetonide 20-hydroxyecdysone of formula found in very small amounts in some plants, e.g. Rhaponticum carthamoides. Method is implemented by interaction of 20- hydroxyecdysone (1.0 g, 2.08 mmole) and acetone with phosphomolybdic acid (PMA) added. As suspension is effected by mother compound in PMA acetone (0.3 g, 0.16 mmole), after 5 min homogenisation of reaction mixture is observed to be steamed by neutralisation with 0.1% sodium hydrocarbonate solution with following ethyl acetate and chromatography extraction of the end product, thus resulting in isolation of the end 2,3-monoacetonide 20- hydroxyecdysone of 32% yield.
EFFECT: method is highly selective and single-stage.
2 cl, 1 ex
SUBSTANCE: claimed invention relates to novel fusidic acid derivatives of general formula [I], where X represents halogen, trifluoromethyl, C1-C7alkyl, substituted with phenyl, C2-C9alkenyl, optionally substituted with C1-C7alkyl, halogen or phenyl, phenyl, optionally substituted with one or two similar or different substituents, selected from group consisting of halogen, C1-C7alkyl, C2-C9alkenyl, phenyl, C1-C6alkoxy, nitro, C1-C6alkyltio, trifluoromethyl and cyano; or X represents naphtyl; Y and Z both represent hydrogen or together with bond C-17/C-20 form double bond between C-17 and C-20 or together represent methylene and form cyclopropane ring in combination with C-17 and C-20; A represents O, S or S(O); B represents C1-6alkyl, C2-6alkenyl, C1-6acyl, phenyl or benzoyl, where C1-6alkyl is optionally substituted with one or more halogens, hydroxy, C2-6alkenyl, phenyl, C1-4heteroaryl or C1-6alkoxy; Q1 represents -(CHOH)-, or -(CHW)-, where W represents halogen or azido; Q2 represents -(CHOH)-; to their pharmaceutically acceptable salts and easily hydrolysed esters and to pharmaceutical compositions, including said derivatives, as well as to their application in therapy.
EFFECT: application in therapy.
31 cl, 127 ex, 5 tbl
FIELD: production processes.
SUBSTANCE: invention refers to wood working and wood chemical industries. Birch bark is broken down, mixed with liquid, the mixture is held at temperature higher than mixture freezing temperature, then triterpene compounds are separated from lingo-adipic residue with the following filtration and drying. Birch bark is additionally broken down by method of impact-abrasing and/or abrasing effect till obtaining birch bark flour. Birch bark flour is mixed with liquid with density of 0.999-0.958 kg/m3. Mixture is held for 0.1-10 hours and then separated by flotation to hydrophobic and hydrophilous fraction. Solution remaining after separation is condensed and dried. Obtained hydrophobic fraction - mixture of triterpene compounds - is exposed to recrystallisation in ethanol with activated charcoal and then betuline, solution of triterpene compounds in ethanol and mixture of triterpene and polyphenol compounds at carbon matrix is obtained. Or triterpene compounds mixture is separated to fractions in carbon-dioxide extractor and betuline, dry mixture of triterpene and polyphenol compounds are obtained. Hydrophilous fraction - lingo-adipic flour - is separated from liquid and dried out.
EFFECT: increase of environmental safety and method effectiveness.
6 cl, 4 ex, 3 dwg
SUBSTANCE: present invention presents a preparation to reduce insulin resistance. The preparation contains 3-O-v-D-glucopyranosyl-4-methylergost-7-ene-3-ole, or an extract made with using an organic solvent, or an extract made with using hot water, or a drained liquid of a plant of Liliaceae family, or fraction thereof which contains this compound as an active component.
EFFECT: production of the preparation which is suitable for inhibition of adipocytokine production, particularly adipocytokine which cause insulin resistance, and for prevention of pathological conditions caused by insulin resistance, or simplification of clinical course of said pathological conditions.
9 cl, 3 ex