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Method for producing ursodesoxycholic acid from 86% of chenodeoxycholic acid

A technology of chenodeoxycholic acid and ursodeoxycholic acid, which is applied in the field of treatment of gallstones and the preparation of liver-protecting drugs, can solve the problems of scarcity of bear bile medicinal materials and low cost, and achieve low cost and low production cost , The effect of easy-to-obtain raw material sources

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

[0005] 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 content 86% of chenodeoxycholic acid through a large amount of groping and test summary; The problem of scarcity of bear bile medicinal materials, and the process of the present invention is simple, low in cost, and improves the purity of androstoxycholic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 10kg of chenodeoxycholic acid with a content of 86%, add 10 times the amount of methanol and dissolve at 60°C for 5 hours, then lower the temperature to 10°C after dissolving, then add 10% bromine solution, and stir at 8°C for 8 hours, Then raise the temperature to 60°C and add 30kg of sodium carbonate, then add 500kg of water to produce a precipitate, filter, crystallize and dry in vacuum at 80°C for 8 hours to obtain 7-ketone; take 10kg of 7-ketone, add 30kg of tert-butanol at temperature Dissolve at 60°C for 2 hours, then add 5kg of sodium metal, stir at 90°C for 2 hours, then stop stirring, filter, and dry the crystals in vacuum at 80°C. Take 10kg of the above dry product, then add 30kg of ethyl acetate, then add 2kg of triethylamine to dissolve at 60°C, and stir for 2 hours, then adjust the pH to about 2.5 with HCL, filter, crystallize, and vacuum dry at 80°C to obtain the purity UDCA above 98.5%.

Embodiment 2

[0031] Take 5 kg of chenodeoxycholic acid with a content of 86% as a raw material, add 6 times the amount of methanol, heat to 60° C., and dissolve for 7 hours;

[0032] Lower the temperature of the dissolved solution to 5°C, then add 7% bromine solution, and react at 5°C for 10 hours;

[0033] Reheat the solution after the above reaction to 50°C, then add 20kg of sodium carbonate, add 400kg of water to filter, discard the filtrate, and dry the crystals under vacuum at 70°C to obtain 7-ketone;

[0034] Take 6kg of the above-mentioned 7-ketone, add 20kg of tert-butanol, heat up to 50°C to dissolve, add 3kg of sodium metal, stir at 70°C for 3 hours, then stop stirring, filter, and vacuum-dry the crystals at 70°C;

[0035] Take 6kg of the above crystalline product, add 20kg of ethyl acetate, then add 0.5kg of triethylamine to dissolve at 40°C, and stir for 3 hours, then adjust the pH to about 2.5 with HCl, filter, discard the filtrate, and dry the crystals in vacuum at 70°C , to...

Embodiment 3

[0037] Take 20 kg of chenodeoxycholic acid with a content of 86% as a raw material, add 15 times the amount of methanol, heat at 70°C, and dissolve for 3 hours;

[0038] Lower the temperature of the above-mentioned dissolved solution to 10°C, then add 12% bromine solution, and react at 10°C for 6 hours;

[0039] Reheat the solution after the above reaction to 60°C, then add 40kg of sodium carbonate, add 650kg of water to filter, discard the filtrate, and dry the crystals under vacuum at 90°C to obtain 7-ketone;

[0040] Take 12kg of the above-mentioned 7-ketone, add 40kg of tert-butanol, heat up to 70°C to dissolve, add 8kg of sodium metal, stir at 100°C for 1 hour, then stop stirring, filter, and dry the crystals in vacuum at 100°C;

[0041] Take 12kg of the above-mentioned crystalline product, add 50kg of ethyl acetate, then add 3kg of triethylamine to dissolve at 75°C, and stir for 1 hour, then adjust the pH to about 2.5 with HCl, filter, discard the filtrate, and dry the c...

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Abstract

The invention relates to a productive process for producing ursodeoxycholic acid by using 86% anthrodsoxycholic acid content, which comprises obtaining ursodeoxycholic acid by using 86% anthrodsoxycholic acid after reaction, and then obtaining ursodeoxycholic acid with 98.5% purity through separating by acetic acid ethyl ester. The productive process has simple technical process and low productive cost. And the purification of ursodeoxycholic acid which is synthesized through adopting bromine as KI oxidant, metallic sodium plus tert-butanol reduction and acetic acid ethyl ester separation is high, which reaches to the international advanced level.

Description

technical field [0001] The invention relates to a preparation method of a medicine for treating gallstones and protecting the liver, in particular to a production method of ursodeoxycholic acid with a content of 86% chenodeoxycholic acid. Background technique [0002] The chemical name of ursodeoxycholic acid is: 3α, 7β-dihydroxy-5β-cholic acid, which has the same molecular formula as chenodeoxycholic acid and bovine cholic acid, but different three-dimensional structures. Chemically, the structures of these two compounds are The relationship is called isomerism. This product is white crystalline powder, odorless, bitter taste. Soluble in ethanol, chloroform, glacial acetic acid, dilute lye, slightly soluble in ether, insoluble in water and dilute mineral acid, melting point 203 ° C, [α]. +57°Ursodeoxycholic acid (UDCA) is a non-toxic hydrophilic cholic acid, which can competitively inhibit the absorption of toxic endogenous cholic acid in the ileum, by activating the sign...

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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