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Method for producing tauro-ursodesoxycholic acid with 98.5 percent ursodesoxycholic acid

A technology of tauroursodeoxycholic acid and ursodeoxycholic acid, applied in the direction of steroids, organic chemistry, etc., can solve the problem of scarcity of bear bile medicinal materials, achieve low production cost, broad market prospects, and easy source of raw materials The effect

Inactive Publication Date: 2013-04-03
辽宁百隆生物工程有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims at the problems existing in the above-mentioned prior art, and through a large amount of groping and test summary, provides a kind of production method of tauroursodeoxycholic acid with content 98.5% ursodeoxycholic acid; Solved existing In the technology, there are problems of scarcity of bear bile medicinal materials and extraction of bile from live bears, and the process of the present invention is simple and low in cost

Method used

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  • Method for producing tauro-ursodesoxycholic acid with 98.5 percent ursodesoxycholic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 50 kg of ethyl acetate and add it to the reaction kettle, then add 4 kg of ursodeoxycholic acid with a content of 98.5%, add 2 kg of triethylamine, and heat for 2 hours to obtain the reaction solution A;

[0014] Cool the above reaction solution A to 10°C, add 2.5 kg of ethyl chloroformate, and reflux for 1 hour to obtain reaction solution B;

[0015] Add 2kg of taurine to the above reaction solution B, add 50kg of water, then add 0.5kg of sodium hydroxide, stir at 10-15°C for 1 hour, add hydrochloric acid to adjust the pH to 2.0, and obtain reaction solution C;

[0016] Transfer the above reaction solution C to another reaction tank, add 50 kg of water, raise the temperature to 30° C., stir for 10 minutes, transfer the reaction solution to a separation tank, let stand for 3 hours, and separate layers.

[0017] The ethyl acetate layer was separated out, and the ethyl acetate was recovered for later use.

[0018] The separated aqueous layer was concentrated to dryn...

Embodiment 2

[0021] Take 70 kg of ethyl acetate and add it to the reaction kettle, then add 8 kg of ursodeoxycholic acid with a content of 98.5%, add 5 kg of triethylamine, and heat for 3 hours to obtain the reaction solution A;

[0022] Cool the above reaction solution A to 15°C, add 5.0 kg of ethyl chloroformate, and reflux for 3 hours to obtain the reaction solution B;

[0023] Add 3kg of taurine to the above reaction solution B, add 60kg of water, then add 1.0kg of sodium hydroxide, stir at 10-15°C for 2 hours, then add hydrochloric acid to adjust the pH to 3.0; the reaction solution C is obtained;

[0024] Transfer the above reaction solution C to another reaction tank, add 70kg of water, raise the temperature to 40°C, stir for 10 minutes, then transfer the reaction solution to a separation tank, let it stand for 4 hours and then separate into layers.

[0025] The ethyl acetate layer was separated out, and the ethyl acetate was recovered for later use.

[0026] The separated aqueous ...

Embodiment 3

[0029] Take 60 kg of ethyl acetate and add it to the reaction kettle, then add 6 kg of ursodeoxycholic acid with a content of 98.5%, add 3 kg of triethylamine, and heat for 2.5 hours to obtain the reaction solution A;

[0030] Cool the above reaction solution A to 13°C, add 3 kg of ethyl chloroformate, and reflux for 2 hours to obtain reaction solution B;

[0031] Add 2.5 kg of taurine to the above reaction solution B, add 55 kg of water, then add 0.8 kg of sodium hydroxide, stir at 13°C for 1.5 hours, add hydrochloric acid to adjust the pH to 2.5; obtain reaction solution C;

[0032] Transfer the above reaction solution C to another reaction tank, add 60kg of water, raise the temperature to 35°C, stir for 10 minutes, then transfer the reaction solution to a separation tank, let it stand for 3.5 hours and then separate into layers.

[0033] The ethyl acetate layer was separated out, and the ethyl acetate was recovered for later use.

[0034] The separated aqueous layer was co...

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Abstract

The invention relates to a method for producing tauro-ursodesoxycholic acid with 98.5 percent ursodesoxycholic acid. The method comprises the following steps: carrying out reaction of 98.5 percent ursodesoxycholic acid, ethyl acetate, ethyl chlorocarbonate, taurine and the like; and obtaining tauro-ursodesoxycholic acid, of which the effective components are the same as those of natural bear bile, through steps including delaminating, filtration, recovery, drying and the like. The method has the advantages that the problems that the herb bear bile is scarce and taking bile from a living bear is difficult are solved; the manufacturing process is simple; the raw material sources are wide; the production cost is low; the production reaches international advanced level; risks in production, transportation and storage are avoided; and the market prospect is wide.

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 tauroursodeoxycholic acid with a content of 98.5% ursodeoxycholic acid. Background technique [0002] Tauroursodeoxycholic acid is an active ingredient of natural bear bile. my country has used bear bile to treat various diseases for thousands of years. Now in order to obtain bear bile powder, we have adopted the method of extracting bile from live bears. Bear bile has been condemned by the international community and also opposed by the broad masses of the people in China. Contents of the invention [0003] The present invention aims at the problems existing in the above-mentioned prior art, and through a large amount of groping and test summary, provides a kind of production method of tauroursodeoxycholic acid with content 98.5% ursodeoxycholic acid; Solved existing In the technology, there are proble...

Claims

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Application Information

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IPC IPC(8): C07J41/00
Inventor 姚凤云刘墨涵
Owner 辽宁百隆生物工程有限公司
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