Method of birch bark processing
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
The invention relates to woodworking and timber industry and can be used to extract valuable chemicals for cosmetics, pharmaceutical and medical industry of waste wood, in particular betulin from birch bark, which is a waste product of the plywood and pulp and paper enterprises.
A method of obtaining natural derivative compounds from birch bark, including soaking bark for from 1 minute to 24 hours at a temperature of from 80°C to 160°C in a composition comprising an organic solvent, extracting natural compounds from birch bark, and chemically active reagent. As the organic solvent used chloroform CHCI3, dichloromethane CH3CI2, diethyl ether (CH3CH2)20, tetrahydrofuran, acetone, pyridine and dimethylformamide DMF.
As a chemically active reagent use nitrates of iron, copper, chromium, zinc, mercury, selenium, manganese, silver, chromium oxide; the chlorides of iron, silver; pyridine chlorochromate RCA peridynamic PDC, K2FeO4To2MnO4, BaMnO4, AgCO3, RuCI, and others. IPC AC 35/78, the description of the invention to the U.S. patent No. 6280778, publ. 28.08.2001,).
The disadvantage of this method is the use of x is mikeski active reagent, in the resulting wastes require disposal in special landfills. The method is complex, characterized by a rather low yield.
A method of obtaining betulin from birch bark, including shredding bark, processing of the crushed mass with a mixture of water-alcohol-alkali when using the shock-acoustic stimulation for 5 minutes at a temperature of 70°C, evaporation of the resulting solution, the precipitation of betulin from one stripped off solution upon dilution with water and subsequent separation of betulin filtering (See. IPC C07J 53/00, the description of the invention to the patent of Russian Federation №2264411, publ. 20.11.2005,).
Shock-acoustic activation intensifies the hydrolysis of birch bark, which in a few minutes turns into a homogeneous mass of brown. However, when the shock-acoustic activation forms a homogeneous mass, not amenable to filtration. Besieged betulin contaminated difficult detachable alkali. Itself percussion-acoustic activation harmful for staff, besides, not provided full use of the components of the bark.
Closest to the claimed method is a method of processing bark for obtaining betulin, including grinding crust on the crusher, the division into the bark and phloem, the extraction of birch bark toluene for 1,53 hours at a temperature of 90-110°C. the filtered solution at a temperature of 40-50°C, the cooling solution of betulin within 6-10 hours to a temperature 15-5°C, stirring precipitated crystals betulin from the mother liquor, filtering, washing with clean toluene, filtration and drying, washing with ethyl alcohol or isopropyl, and then with water, and the final drying (See. IPC AC 35/78, SN 5/04, description of invention to the patent of Russian Federation №2192879, publ. 20.11.2002, the Nearest equivalent).
The disadvantages of this method are:
- the complexity of the technological process, especially at the stage of mixing bark with toluene, resulting in a persistent, poorly filterable emulsion;
- high cost-of-way caused by the use of pure expensive and hazardous solvents;
- low degree of sustainability in General and also related to the fact that when the temperature of the filter 40-50°C betulin begins to fall out of the toluene and to crystallize in the pipes, which hinders the extraction process;
- high okolnosti caused by the inability of the complex extract of the bark of various natural derivative compounds.
The technical result of the claimed method of processing bark is to increase process efficiency and environmental safety.
The essence of the technical solution is the method of processing of birch bark, including shredding bark, mixing it with liquid, maintaining the mixture at a temperature above freezing mixture, bark additionally crushed by the method of shock-abrasive effects to get birch bark flour, which is mixed with the liquid density 0,999-0,958 kg/m3the mixture was incubated for 0.1 to 10 hours and share flotation on hydrophobic and hydrophilic fractions of the hydrophilic fraction is separated from the liquid and dried to obtain ligno-fat flour, obtained from the hydrophobic fraction is a mixture of triterpene compounds separated crystals are washed, dried and subjected to recrystallization in ethanol with activated charcoal and get betulin, a solution of triterpene compounds in ethanol and a mixture of triterpene and polyphenolic compounds in the coal matrix, the solution remaining after separation of the crystals is thickened or dried with getting polyphenolic extract or separated into fractions in carbon dioxide extractor and get betulin, a dry mixture of triterpene and polyphenolic compounds, the solution remaining after separation of the crystals is thickened or dried with getting polyphenolic extract, with shredding bark is carried out in a planetary mill in the camera planetary mill serves fluid, as grinding media in the grinding circuit using corundum and/or is the club include, crystals triterpene compounds washed with distilled water.
Additional shredding bark method of shock-abrasive exposure it is possible to obtain fine flour with broken chemical bonds in polymers bark, and gives the property to absorb water unlike the original birch bark and extract from it the maximum amount of valuable substances. A new property of the obtained material allows you to select triterpene fraction, due to its hydrophobicity, by flotation.
In addition, it allows for the extraction of triterpene compounds as liquid water without the use of such environmentally hazardous solvents, such as, for example, azeotropic mixture of tetrachloroethylene - water.
These parameters fluid density, the ratio of bark flour and liquid, temperature and exposure time are optimal for the efficiency of the process and are interrelated. Thus, when fluid density below 0,958 kg/m3, temperatures above 100°C and holding time of less than 0.1 hour, the resulting mixture was badly divided into hydrophobic and hydrophilic fractions. Hydrophobic fraction is a triterpene fraction of birch bark, which is due to the hydrophobicity POPs up and hydrophilic fraction - ligno-fat fraction, which absorb moisture and sink.
When pre is ysenia above the upper boundary of the process parameters is impractical, because the mixture is not fractions.
Washing crystals triterpene compounds distilled water helps get rid of ballast substances, such as tannins, polysaccharides, and other.
Additional introduction into the chamber of the planetary mill fluid increases the efficiency of the abrasive impact due to more snug fit flour to the grinding bodies and intensifies the process of saturation of the liquid hydrophilic fraction.
The allocation of betulin from a mixture of triterpene compounds by recrystallization in ethanol with activated carbon or by dividing into factions in carbon dioxide extractor allows to obtain pure betulin content of the main substance of 97% and above. Recrystallization in ethyl alcohol also allows to obtain in a single technological cycle advanced solution triterpene compounds in ethanol and a mixture of triterpene, and other polyphenolic compounds in the coal matrix, used as cosmetic, pharmaceutical and veterinary products and/or raw materials. Processing a mixture of triterpene compounds in carbon dioxide extractor allows you to get pure betulin and a mixture of triterpene compounds used in the future as cosmetic, pharmaceutical and veterinary the drugs and/or raw materials without the use of liquids and, therefore, no process steps such as filtering, drying and regeneration of the solvent.
The inventive method of processing bark is illustrated operational algorithm of the method, where:
figure 1 shows the sequence of operations of a way to get bark flour, a mixture of triterpene compounds, polyphenolic extract and ligno-fat balance;
figure 2 - sequence of operations for obtaining betulin by recrystallization;
figure 3 - sequence of operations for obtaining betulin in carbon dioxide extractor.
A method of processing bark is as follows. Take cleansed from impurities (pieces of wood) bark, ground in a knife mill or a hammer mill to a particle size of about 1.0×1,0×1,0 mm and then in the device, where the shock-abrasive impact, such as a planetary mill, with a ratio of rotational speeds of the drum and drove from 0.3 to 0.7, as the grinding media used corundum and/or Jasper, the bark is crushed to obtain birch bark flour, which is mixed, for example, water density of 0,958 to 0,999 kg/m3. The mixture was incubated until saturation of the liquid hydrophilic fraction and served on the flotation device, such as a mechanical flotation machine, inwhich instead of air is used, carbon dioxide or other inert gas to avoid oxidation of target products. The flotation device is divided suspension of hydrophobic fraction triterpene compounds (mixture of triterpene compounds and hydrophilic ligno-fat fraction (ligno-fat meal). Hydrophobic fraction is separated from the liquid, for example, by filtration, the filtrate is washed with distilled water and dried or recrystallized in ethanol with activated carbon, or separated into fractions in carbon dioxide extractor. The obtained crystals betulin is filtered off and dried. The result is betulin in the form of a white powder with a yield up to 35% of the weight loaded in the planetary mill bark and purity of 97%. The mother liquor solution triterpene compounds in ethanol use as a cosmetic, pharmaceutical or veterinary facility.
EXAMPLE 1. Crushed to a fraction of 1,0×1,0×1,0 bark in the amount of 100 kg load in the planetary mill as the grinding media used corundum, and is subjected to its shock-abrasion when the ratio of the speeds of rotation of the drums, and led, equal to 0.4. Obtained birch bark flour is mixed with water in an amount of 550 kg density 0,999 kg/m3the mixture was incubated for 10 hours. Then, after separating a mixture of mechanical flotation machine, the mixture of triterpene compounds washed distil the new water in an amount of 60 l, dried and sent for recrystallization in ethanol with activated carbon at a temperature of the boiling mixture in the ratio of mixture of triterpene compounds coal 1-5-0,5, respectively. As a result of recrystallization is a selection of betulin from a mixture of triterpene compounds, which is filtered off from the mother liquor and dried in a dryer at a temperature of from 80 to 200°C. and a pressure of from 0.01 to 0.1 MPa to remove ethanol. Get up to 25% of betulin 97% purity. Ligno-fat flour is separated from the liquid and dried, separated mixture is a polyphenolic extract, which is used without processing, or thickened, or dried by any known method.
EXAMPLE 2. Take 100 kg of milled bark and load in the planetary mill as grinding media is used corundum and Jasper, and subjected to its shock-abrasion when the ratio of the speeds of rotation of the drums, and led, equal to 0.55, exposes its shock-abrasion. In the grinding chamber, water is supplied in a quantity of 50 kg at ambient temperature, the mixture birch bark flour and water, water is added in the amount of 550 kg density 0,958 kg/m3. The mixture was incubated for 1 hour. Further, the process is carried out analogously to example 1. Get up to 29% betulin 97% purity.
P the EMER 3. Take 100 kg of milled bark and load in the planetary mill as grinding media use Jasper. The bark is subjected to shock-abrasion when the ratio of the speeds of rotation of the drums and was taken equal to 0.7. In the resulting bark flour, water is added in the amount of 650 kg density 0,958 kg/m3at boiling point. The resulting mixture was incubated for 0.1 hours. After washing the triterpene fraction distilled water in an amount of 10 l, it is dried and Packed or placed in a carbon dioxide extractor, which is the final separation of impurities from betulin, betulin remains in the extractor. After this transaction, the company does not require additional drying. The output of betulin is up 31%.
EXAMPLE 4. Take 100 kg of crushed bark, load in the planetary mill as the grinding media used corundum, in the grinding chamber serves 50 kg liquid which is a mixture of water-ethanol density 0,959 kg/m3. After grinding add the specified fluid in the amount of 500 kg of the Mixture was kept for 1 hour. Further, the process is carried out analogously to example 1. Use as a liquid mixture of water - ethanol allows the use of an unheated room at negative ambient temperatures.
As the liquids and can be used a mixture of: water-ethyl alcohol, water-isopropyl alcohol density 0,999-0,958 kg/m3.
The proposed method for processing bark is complex, while the simplicity and adaptability of environmentally safe. The products obtained, namely a mixture of triterpene compounds, betulin, bark flour, solution triterpene compounds in ethyl alcohol and polyphenolic extracts are valuable raw materials for food, pharmaceutical and perfumery industry and environmentally safe. In addition, bark flour can be packaged and used in raw form for use in food, cosmetic, pharmaceutical and veterinary industries.
The method does not require the use of chemically active fluids, which reduces the level of environmental hazard for maintenance personnel and for the environment by reducing waste toxicity.
1. The method of birch bark processing, including grinding bark, mixing it with liquid, maintaining the mixture at a temperature above freezing mixture, characterized in that the bark additionally crushed by the method of shock-abrasive effects to get birch bark flour, which is mixed with the liquid density 0,999-0,958 kg/m3the mixture was incubated for 0.1-10 h, and share flotation on hydrophobic and hydrophilic fractions of hydrophilic fra is tion is separated from the liquid and dried to obtain lisnagarvey flour, from the obtained hydrophobic fraction is a mixture of triterpene compounds separated crystals are washed, dried and subjected to recrystallization in ethanol with activated charcoal and get betulin, a solution of triterpene compounds in ethanol and a mixture of triterpene and polyphenolic compounds in the coal matrix, the solution remaining after separation of the crystals, condensed or dried with getting polyphenolic extract.
2. The method of birch bark processing, including grinding bark, mixing it with liquid, maintaining the mixture at a temperature above the freezing temperature of the mixture, characterized in that the bark additionally crushed by the method of shock-abrasive effects to get birch bark flour, which is mixed with water density 0,999-0,958 kg/m3the mixture was incubated for 0.1-10 h, and share flotation on hydrophobic and hydrophilic fractions of the hydrophilic fraction is separated from the liquid and dried to obtain lisnagarvey flour, obtained from the hydrophobic fraction is a mixture of triterpene compounds separated crystals are washed, dried, separated into fractions in carbon dioxide extractor and get betulin, a dry mixture of triterpene and polyphenolic compounds, the solution remaining after separation of the crystals, condensed or dried with getting polyphenolic extract.
3. The way p is rerabotka bark according to claim 1 or 2, characterized in that the grinding bark is carried out in a planetary mill.
4. A method of processing bark according to claim 3, characterized in that during grinding in the planetary camera of the mill serves fluid.
5. A method of processing bark according to claim 4, characterized in that as the grinding media in the grinding circuit using corundum and/or Jasper.
6. A method of processing bark according to claim 5, characterized in that the crystals triterpene compounds washed with distilled water.
FIELD: medicine; virology.
SUBSTANCE: claimed is application of birch bark extract as adjuvant. Invention can be used in veterinary and medicine.
EFFECT: birch bark extract increases immunogenity of target antigen in combined introduction.
3 cl, 4 tbl, 4 ex
FIELD: chemical technology.
SUBSTANCE: invention relates to chemical processing wood. Ligno-containing raw as air-dried saw-dust is treated with ammonium persulfate aqueous solution at temperature 60oC under conditions of cavitation treatment in rotor-pulsed device at the rotor revolution rate 3000 rev/min/. Treatment is carried out for 0.25-1.0 h at the concentration of ammonium persulfate 0.2-0.8 g/g of raw and at the concentration of ammonia 0.5-2.0 wt.-%. Method provides decreasing the ammonium consumption and peroxy-compound as an oxidant, duration of the process that allows decreasing cost of the technological process. High-molecular materials prepared by the proposed method comprise up to 4.3% of bound nitrogen. About 17-25% of bound nitrogen is released as ammonium at acid and alkaline hydrolysis, and the remained amount of nitrogen is tightly bound with wood. Nitrogen-containing materials comprise up to 6.8% of carboxyl groups and 20.5% of lignin. Invention provides decreasing consumption of ammonium persulfate by 7.5-9 times, decreasing the concentration of ammonium up to 0.5-2.0 wt.-% and declining of the process period from 2 to 0.25-1 h. Invention can be used for preparing nitrogen-containing fertilizers and sorbents based on ligno-carbohydrate raw.
EFFECT: improved preparing method.
4 tbl, 10 ex
FIELD: chemistry of natural compounds.
SUBSTANCE: processing comprises isolation of betulin from ground bark via extraction with organic solvent within closed extraction technological complex. Extraction is effected in flow-type extractor at solvent boiling temperature while continuously withdrawing extract to evaporation still and solvent vapors from extractor and from evaporation still to condenser. Solvent vapors are condensed and condensate is recycled. Betulin, if necessary, is purified. Extracted bark is treated, at heating and stirring, with water-alcohol alkali solution, which is not being removed from extractor. Hot reaction mass is then filtered to obtain non-dissolved cellolignin and filtrate containing suberic acid sodium salts. Filtrate is evaporated and simultaneously clarified with hydrogen peroxide.
EFFECT: enabled easily obtaining betulin and sodium suberate on the same installation and in the same cycle.
7 cl, 1 dwg, 1 tbl, 18 ex
FIELD: natural substances technology.
SUBSTANCE: method of preparing extractive substances from ground birch bark comprises extraction and filtration of precipitated extract. Extraction is effected with extractant condensate sprinkling ground birch bark bed in presence of ascending vapors of the same extractant. Extractant is two-component mixture of water and low-boiling solvent having boiling point below 100°C. Product is isolated by bringing extractant condensate containing dissolved extract with contents of receiver. Once extraction is completed, solvent is removed with live steam.
EFFECT: reduced consumption of extractant, increased degree of extractant regeneration, simplified isolation of product, and reduced fire and explosion risk.
1 tbl, 2 ex
FIELD: resin industry.
SUBSTANCE: method is designed for use in fabrication of plastics and composites with mineral and organic fillers. Method of invention comprises treating initial material with acetic anhydride in presence of catalyst at a ratio of 0.5-3.0 mole anhydride per 1 mole hydroxyl groups of material at intensive mechanical division of reaction mixture for 0.5 to 3 h at 25°C, said catalyst being ammonium sulfate used in amount 5-30% of the mass of lignohydrocarbon material.
EFFECT: reduced consumption of reagents by a factor 3 to 10, reduced duration of process to 1-3 h at temperature lowered to 25°C, and reduced process expenses.
4 tbl, 19 ex
FIELD: industrial organic synthesis.
SUBSTANCE: invention concerns preparation of sodium salts of sulfate esters of lingo-carbohydrate materials, which can be used as chemical additives to control properties of washing fluids used in boring oil and gas wells. Method of preparing water-soluble sulfuric acid esters of cellulose-based lingo-carbohydrate materials consists in that material is activated with sodium hydroxide and then affected by sodium fluorosulfonate. Activation of mechanically divided lingo-carbohydrate material composed of non-preliminarily separated cellulose, lignin, and hemicelluloses is conducted for 1 h at 70°C and reaction is carried out in isopropyl alcohol fir 3-15 h at 50-90°C and molar ratio of lingo-carbohydrate material to sodium fluorosulfonate equal to 1:(1-1.75).
EFFECT: enabled utilization of total amount of lingo-carbohydrate material, reduced price cost of final product, improved environmental condition, and widened spectrum of properties of final product.
4 tbl, 15 ex
FIELD: method for production of carboxymethyl esters useful as adsorbents.
SUBSTANCE: claimed method includes preliminary removing from air-dry lignocarbohydrate material of extractive and water soluble substances by 3-steps subsequent extraction with alcohol/benzene mixture, hot water and cold water. Then macromolecules are cross-linked by polycondensation of extracted material with formaldehyde in ratio lignocarbohydrate material OH-groups/formaldehyde of 1:3-5 in presence of alkali catalyst. Cross-linked lignocarbohydrate material is washed and carboxymethylated with monochloroacetic acid and alkali in ratio lignocarbohydrate material OH-groups/ClCH2COOH/NaOH of 1:3:27 at 45-65°C for at least 3 h. Obtained product is separated, treated with mineral acid to convert carboxylic groups to H-form; washed with water up to neutral filtrate pH-value, and dried.
EFFECT: product with high content of carboxylic groups, increased change capacity, and stability in aqueous and non-aqueous media.
6 ex, 2 tbl
FIELD: chemical wood reprocessing, in particularly for production of nitrogen-containing fertilizers and sorbents based on lignocarbohydrate raw material.
SUBSTANCE: claimed method includes treatment of lignin-containing raw material with ammonium solution of peroxide compound (e.g., hydrogen peroxide) containing 0.03-0.9 of hydrogen peroxide and 0.25-1.5 g of ammonium (in respect to 1 g of raw material), while thorough mechanical grinding at 20°C, frequency of 2800 cm-1,for 0.25-2.0 h. Method of present invention makes it possible to reduce oxidizing agent consumption by 4-5 times and ammonium amount by 1,5 times.
EFFECT: method with decreased reagent consumption and reduced process durability.
22 ex, 4 tbl
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
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 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: 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
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
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: 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, 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
SUBSTANCE: invention concerns medicine area, namely to gynecology and concerns a non-operative way of treatment of hysteromyoma. For this purpose wearing of loose leaves "Piokal" for 8-15 hours a day within 6-9 months is prescribed to the patient. Biologically active additive to nutrition "Beloyar with calendula extraction" after 1-2 dining rooms of a spoon 3 times a day before meal, a course of 10-30 days is simultaneously entered. In the presence of cardiovascular system diseases it is entered "Beloyar with hawthorn extraction", and in case of presence of an allergy and the lowered immunity - "Beloyar with licorice extraction". In addition "Chitovit" is entered on 1-2 tablet 3 times a day within 10-15 days. From the first day of a menstrual cycle 2-3 times a day the "Migs" are prescribed within 15 days on1 table-spoon. DS "Dobrodeya" is entered into second half of an ovarian-menstrual cycle, 30 minutes prior to food intake 2-3 times a day within 15 days - two cycles successively for women that are younger than 40 years, and for women that are older than 40 years or in the presence of an accompanying pathology - three cycles successively. During a break between cycles reception of "Lokhelan" 20-30 minutes prior to meal on a quarter of a glass 2 times a day, course of treatment - 20 days, 2-4 times a year is prescribed. It is possible to repeat the course 2-3 times a year. Term of treatment of hysteromyoma makes 6-12 months.
EFFECT: elimination of chronic hypoxia of a brain, normalisation of hypothalamo-pituitary-adrenal axis function, provision of reduction of the sizes of myoma, prevention of disease relapses.