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Purification method of ursodesoxycholic acid

A technology of ursodeoxycholic acid and a purification method, which is applied in the field of purification of ursodeoxycholic acid, can solve the problems of huge energy consumption, large amount of solvent used, and low production capacity in the solvent recovery step, and achieve easy operation and simple solvent The effect of gaining and low energy consumption

Active Publication Date: 2017-07-07
眉山市新功生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally speaking, using ethyl acetate as a solvent, the production capacity per unit of solvent is low, the amount of solvent used is large, and the subsequent solvent recovery steps consume a lot of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Preparation of ursodeoxycholic acid triethylamine salt

[0035] 100g (80% ursodeoxycholic acid content) crude product was added successively with 6 times the volume of acetone 600mL, 0.5 times the volume of ethanol 50mL and stirred to raise the temperature to 46°C, and maintain the temperature for 1.5 hours; add 1 times the volume of triethylamine 100mL again, and heat up Reflux for 1.5 hours to react ursodeoxycholic acid with triethylamine to form ursodeoxycholic acid triethylamine salt; slowly cool down to 14°C, stir and react for 4 hours; filter, wash the filter cake with 100 mL of acetone of 1 volume, The wet product ursodeoxycholic acid triethylamine salt 130.7g was obtained.

[0036] 2. Hydrolysis of ursodeoxycholic acid triethylamine salt

[0037] Put the appealing filter cake into the reaction bottle, add 10 times the volume of acetone 1000mL, 3 times the volume of water 300mL, stir and raise the temperature to 46°C, and maintain the temperature for half an ...

Embodiment 2

[0045] 1. Preparation of ursodeoxycholic acid triethylamine salt

[0046]100g (82% ursodeoxycholic acid content) crude product was added successively with 6 times the volume of acetone 600mL, 0.5 times the volume of ethanol 50mL and stirred to raise the temperature to 45°C, maintaining the temperature for 2 hours; adding 1 times the volume of triethylamine 100mL again, and heating Reflux for 2 hours to react ursodeoxycholic acid with triethylamine to form ursodeoxycholic acid triethylamine salt; slowly cool down to 10-15°C, stir and react for 4 hours; Cake, obtain wet product ursodeoxycholic acid triethylamine salt 130.6g.

[0047] 2. Hydrolysis of ursodeoxycholic acid triethylamine salt

[0048] Put the above-mentioned filter cake into the reaction bottle, add 10 times the volume of acetone 1000mL, and 3 times the volume of water 300mL, stir and heat up to 45°C, and maintain the temperature for half an hour; after it is completely dissolved, add dropwise glacial acetic acid ...

Embodiment 3

[0056] 1. Preparation of ursodeoxycholic acid triethylamine salt

[0057] 100g (ursodeoxycholic acid content 79%) crude product was successively added 6 times volume of acetone 600mL, 0.5 times volume of ethanol 50mL and stirred to raise the temperature to 50°C, maintaining the temperature for 1 hour; adding 1 times volume of triethylamine 100mL again, heating Reflux reaction for 1-2 hours to make ursodeoxycholic acid react with triethylamine to form ursodeoxycholic acid triethylamine salt; slowly cool down to 10-15°C, stir and react for 4 hours; filter, 100 mL of acetone with 1 volume Wash the filter cake to obtain the wet product ursodeoxycholic acid triethylamine salt 130.2.

[0058] 2. Hydrolysis of ursodeoxycholic acid triethylamine salt

[0059] Put the appealing filter cake into the reaction bottle, add 10 times the volume of acetone 1000mL, 3 times the volume of water 300mL, stir and heat up to 50°C, and maintain the temperature for half an hour; after it is completel...

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PUM

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Abstract

The invention discloses a purification method of ursodesoxycholic acid. The method comprises the following steps: firstly, preparing a triethylammonium ursodesoxycholicate; secondly, hydrolyzing the triethylammonium ursodesoxycholicate; and finally, performing recrystallization and refining. The purification method of ursodesoxycholic acid disclosed by the invention is simple in step and easy to operate. The used solvent is simple and easily available, and small in energy consumption. The purity of the refined ursodesoxycholic acid obtained by the purification method reaches up to 99.8%.

Description

technical field [0001] The invention relates to the field of medicine separation, in particular to a method for purifying ursodeoxycholic acid. Background technique [0002] Ursodeoxycholic acid (Ursodeoxycholic acid, UDCA, 3α, 7β-dihydroxy-5β-cholestane-24-acid), is the main active ingredient of the precious traditional Chinese medicine bear bile, and it is the main active ingredient in the treatment of primary biliary cirrhosis (PBC). ) the only drug. Clinical application at home and abroad proves that ursodeoxycholic acid has a good curative effect in treating various gallbladder diseases, liver diseases and various hyperlipidemia diseases, especially in dissolving cholesterol gallstones. In recent years, some new curative effects have been discovered. Such as cell protection, immune regulation, anticancer and so on. [0003] Given the importance of ursodeoxycholic acid, there is an increasing demand for its clinical application. However, the natural ursodeoxycholic ac...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 梁万超蒋先曲
Owner 眉山市新功生物科技有限公司
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