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Method for producing chenodeoxycholic acid by using 98.5% sodium cholate

A technique for chenodeoxycholic acid and bovine bile acid, which is applied in the field of preparation of chenodeoxycholic acid, can solve the problems of low purity of chenodeoxycholic acid, few sources of poultry bile, complicated process, etc., and achieves low cost , the effect of low production cost and simple production process

Inactive Publication Date: 2013-03-13
辽宁百隆生物工程有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purity of chenodeoxycholic acid obtained from poultry gall is not high, the process is complicated, and the source of poultry gall is less, which cannot meet people's requirements

Method used

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  • Method for producing chenodeoxycholic acid by using 98.5% sodium cholate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 25 kg of bovine and sheep cholic acid with a content of 98.5%, add 50 kg of methanol, heat and reflux for 1 hour, place at room temperature until crystals form, filter, wash the crystals with 90-120 petroleum ether, dry the crystals in vacuum at 70°C to obtain a dry product, and then Take 2kg of dry product, 10kg of toluene, and 2kg of pyridine and put them into the reaction tank together, stir at room temperature for 40 minutes, then add 120kg of water and stir again for 45 minutes, then stand still for 5 hours, separate the toluene for recovery, and precipitate crystals , crystallization with 90-120 petroleum ether repeatedly washed to obtain 3α, 7α-diacetylcholic acid methyl ester, vacuum drying at 70 ° C, take 1.5 kg of dried 3α, 7α-diacetylcholic acid methyl ester and add 2 kg of acetic acid Sodium, then take 10kg of methanol and put it into the reaction tank together for reflux for 30 minutes, then lower the temperature to 5°C, add 1kg of sodium hypochlorite, ...

Embodiment 2

[0017] Take 60kg of methanol, add 25kg of cholic acid with a content of more than 98.5%, heat and reflux for 1.5 hours, place at room temperature until crystals precipitate, filter, wash with model 90-120 petroleum ether, and vacuum dry at 70°C to obtain methyl cholic acid;

[0018] Get 15kg of toluene, add 3kg of pyridine and add 3kg of the above-mentioned crystallized methyl cholate and stir at room temperature for 50 minutes, then add 140kg of water, stir again for 40 minutes, after standing for 6 hours, separate the toluene and reclaim it, crystallize out, and crystallize in Vacuum drying at 70°C; crystallization was repeatedly washed with 85% petroleum ether of type 90-120 to obtain 3α, 7α-diacetylcholic acid methyl ester.

[0019] Take 3 kg of the above-mentioned 3α, 7α-diacetylcholic acid methyl ester, add 3 kg of sodium acetate, add 12 kg of methanol to reflux for 30 minutes, add 2 kg of sodium hypochlorite when the temperature reaches 8 ° C, continue stirring for 5 hou...

Embodiment 3

[0022] Take 58kg of methanol, add 28kg of bovine and sheep cholic acid with a content of 98.5%, heat and reflux for 2 hours, place at room temperature for 8 hours until crystals precipitate, filter, wash with model 90-120 petroleum ether, and dry under vacuum at 70°C to obtain cholic acid Methyl ester;

[0023] Get 19kg of toluene, add 3kg of pyridine and drop into the reaction kettle, add 3kg of the above-mentioned crystallized methyl cholate and stir at room temperature for 50 minutes, then add 140kg of water, stir again for 40 minutes, after standing for 6 hours, separate the toluene and reclaim it. Crystals were precipitated and dried in vacuum at 70°C; the crystals were washed repeatedly with 90-120 petroleum ether to obtain 3α, 7α-diacetylcholic acid methyl ester.

[0024] Take 3 kg of the above-mentioned 3α, 7α-diacetylcholic acid methyl ester, add 3 kg of sodium acetate, add 11 kg of methanol to reflux for 30 minutes, add 3 kg of sodium hypochlorite when the temperatur...

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Abstract

The invention relates to a method for producing chenodeoxycholic acid by using 98.5% sodium cholate. The method comprises the steps of conducting esterification, acetylation and the like on sodium cholate, converting cholic acid with isomeride into a chenodeoxycholic acid structure so as to form a chenodeoxycholic acid compound, then purifying the chenodeoxycholic acid compound, and separating to obtain chenodeoxycholic acid with the purity of 98.5%. According to the production method, the process is simple, the production cost is low, the problems that the avian bile amount is few and is difficult to collect can be solved, and the internal advanced level is achieved.

Description

technical field [0001] The invention relates to a method for preparing chenodeoxycholic acid, in particular to a method for producing chenodeoxycholic acid with a content of 98.5% of bovine and sheep cholic acid; it is a medicine for dissolving cholesterol stones and is also used for Liver-protective drugs for the treatment of primary biliary cirrhosis (PBS), chronic hepatitis C, alcoholic liver disease, and non-alcoholic 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 gallsto...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 姚凤云刘墨涵
Owner 辽宁百隆生物工程有限公司
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