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Method for producing ursodesoxycholic acid from 98.0% of cholic acid of cattle and sheep

A technology of ursodeoxycholic acid and bovine and sheep cholic acid, which is applied in the field of preparation of ursodeoxycholic acid, can solve the problem of scarcity of bear bile medicinal materials, achieve low cost, low production cost, and solve the effects of scarce medicinal materials

Inactive Publication Date: 2008-07-09
辽宁百隆生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the problems existing in the above-mentioned prior art, and provides a kind of production method of ursodeoxycholic acid with the content of 98.0% bovine and sheep cholic acid through a large amount of groping and test summary; The problem of scarcity of bile medicinal materials, and the process of the present invention is simple, low in cost, improves the purity of androstoxycholic acid, and is suitable for mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 15 kg of bovine and sheep cholic acid, add 40 kg of methanol, heat and reflux for 1 hour, place at room temperature until crystals form, filter, wash the crystals with petroleum ether (model 90-120), dry the crystals in vacuum at 70°C, and then take Take 2kg of dry product, take 10kg of toluene and 2kg of 4-xylylpyridine and put them into the reaction tank together, stir at room temperature for 30 minutes, then add 100kg of water and stir for another 30 minutes, then let stand for 4 hours, separate the toluene for recovery , precipitated crystals, crystallization was repeatedly washed with petroleum ether (model 90-120) to obtain 3α, 7α-diacetylcholic acid methyl ester, vacuum-dried at 80°C, took 1.5kg of dry product, added 2kg of sodium acetate, and then took 10kg of methanol Put them together in the reaction tank and reflux for 30 minutes, then lower the temperature to 5-10°C, add 1kg of bromine solution, continue to stir for 4 hours, then add 100kg of water, cont...

Embodiment 2

[0030] Take 20 kg of methanol, add 5 kg of bovine cholic acid with a content of more than 98.0%, heat and reflux for 0.5 hours, place at room temperature until crystals precipitate, filter, wash with petroleum ether (type 90-120), and vacuum dry at 60°C to obtain methyl cholate;

[0031] Take 5kg of toluene, add 1kg of 4-lutidine, add 1kg of the crystallized methyl cholate and stir at room temperature for 20 minutes, then add 80kg of water, stir again for 20 minutes, then let stand for 2 hours, separate the toluene and then recover , crystals were precipitated, and the crystals were vacuum-dried at 60°C; the crystals were washed repeatedly with petroleum ether (model 90-120) to obtain 3α, 7α-diacetylcholic acid methyl ester;

[0032] Take 0.5 kg of the above methyl diacetyl cholate, add 1 kg of sodium acetate, add 5 kg of methanol to reflux for 20 minutes, add 0.5 kg of bromine solution when the temperature reaches 5 ° C, continue stirring for 2 hours, then add 80 kg of water,...

Embodiment 3

[0040] Take 60 kg of methanol, add 30 kg of bovine and sheep cholic acid with a content of more than 98.0%, heat and reflux for 2 hours, place at room temperature until crystals precipitate, filter, wash with petroleum ether (model 90-120), and vacuum dry at 80 ° C to obtain methyl cholate;

[0041] Take 20kg of toluene, add 4kg of 4-lutidine, add 4kg of the above crystallized methyl cholate, stir at room temperature for 50 minutes, then add 150kg of water, stir again for 50 minutes, then stand still for 6 hours, separate the toluene and recover , crystals were precipitated, and the crystals were vacuum-dried at 100°C; the crystals were washed repeatedly with petroleum ether (model 90-120) to obtain 3α, 7α-methyl diacetylcholic acid;

[0042] Take 4kg of the above-mentioned methyl diacetylcholate, add 4kg of sodium acetate, add 15kg of methanol and reflux for 40 minutes, add 2.5kg of bromine solution when the temperature reaches 10°C, continue stirring for 5 hours, then add 12...

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Abstract

The invention relates to a productive process for producing ursodeoxycholic acid by using 98.0% bovine and sheep cholic acid, which comprises conducting four steps of esterification, acetylization, oxidization and reduction for bovine and sheep cholic acid, transforming cholic acid with isomer into the structure of anthrodsoxycholic acid to form the compound of anthrodsoxycholic acid, obtaining ursodeoxycholic acid after reaction through utilizing anthrodsoxycholic acid, separating to obtain ursodeoxycholic acid with 98.5% purity by utilizing acetic acid ethyl ester. The productive process has simple technical process, low productive cost, and solves the problems of less fowl gall quantity and difficult collection. And the purity of ursodeoxycholic acid which is synthesized is high, which reaches to the international advanced level.

Description

technical field [0001] The present invention relates to a method for preparing ursodeoxycholic acid, in particular to a method for producing ursodeoxycholic acid with a content of 98.0% bovine and sheep cholic acid; it is a medicine for dissolving cholesterol gallstones and is also used for treating Hepatoprotective drugs for primary biliary cirrhosis (PBS), chronic hepatitis C, alcoholic liver disease, and nonalcoholic fatty liver. Background technique [0002] As early as 1848, the active ingredient chenodeoxycholic acid was first discovered in goose bile, and it was named chenodeoxycholic acid (CDCA) in 1924. Since 1937, some people have tried to dissolve gallstones with a mixture containing chenodeoxycholic acid, and later found that chenodeoxycholic acid has the effect of correcting cholesterol-saturated bile. Britain officially opened up the treatment of dissolving cholesterol gallstones in 1972, as the first A drug that corrects saturated bile and dissolves gallstone...

Claims

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Application Information

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IPC IPC(8): C07J9/00C07J75/00
Inventor 姚凤云
Owner 辽宁百隆生物工程有限公司
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