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Fine purification method for cholic acid crude product

A refining method and technology for crude products, which are applied in the fields of steroids, digestive system, organic chemistry, etc., can solve the problems of poor refining effect and complicated operation of cholic acid refining method, and achieve good refining effect, easy mass production and operation. simple effect

Active Publication Date: 2009-10-07
苏州天绿生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for refining the crude product of cholic acid, which solves the problems of complex operation and poor refining effect in the prior art.

Method used

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  • Fine purification method for cholic acid crude product
  • Fine purification method for cholic acid crude product
  • Fine purification method for cholic acid crude product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The refining of embodiment 1 cholic acid crude product

[0035] Get crude product cholic acid 1Kg, cholic acid content is 70%. Add 7:1 glacial acetic acid, stir, soak for 8 hours, and filter. Acetic acid was recovered from the filtrate, and the precipitate was dried to obtain 780 g of cholic acid product A, with a content of 82%.

[0036] Take product A of cholic acid, add 10% triethylamine aqueous solution according to 5:1, stir and soak. filter. Add dilute sulfuric acid to the filtrate to adjust the pH to 2-3. Filter and wash with water until neutral. Get the wet product cholic acid B product.

[0037] Take the wet cholic acid product B, add 95% ethanol in a ratio of 1.5:1, mix, heat to reflux, filter, let cool, and let stand. filter. dry. Obtain fine cholic acid 490g. The detection content is 98.9%

Embodiment 2

[0038] The refining of embodiment 2 cholic acid crude product

[0039] Get crude product cholic acid 1Kg, cholic acid content is 57%. Add 70% acetic acid aqueous solution of 7:1, stir, soak for 8 hours, and filter. Acetic acid was recovered from the filtrate, and the precipitate was dried to obtain 630 g of cholic acid product A, with a content of 75%.

[0040] Take cholic acid product A, add 15% triethylamine aqueous solution according to 5:1, stir and soak. filter. Add dilute sulfuric acid to the filtrate to adjust the pH to 2-3. Filter and wash with water until neutral. Get the wet product cholic acid B product.

[0041] Take the wet product of cholic acid B, add 75% ethanol in a ratio of 1.5:1, mix, heat to reflux, filter, let cool, and let stand. filter. dry. 380g of refined cholic acid was obtained, with a content of 98.9%.

Embodiment 3

[0042] The refining of embodiment 3 cholic acid crude product

[0043] Get crude product cholic acid 1Kg, cholic acid content is 79%. Add 3:1 glacial acetic acid, stir, soak for 8 hours, and filter. Acetic acid was recovered from the filtrate, and the precipitate was dried to obtain 795 g of cholic acid product A, with a content of 84%.

[0044] Take product A of cholic acid, add 7% triethylamine aqueous solution according to 5:1, stir and soak. filter. Add dilute sulfuric acid to the filtrate to adjust the pH to 2-3. Filter and wash with water until neutral. Get the wet product cholic acid B product.

[0045] Take the wet product of cholic acid B, add 99% ethanol in a ratio of 5:1, mix, heat to reflux, filter, let cool, and let stand. filter. dry. 503g of fine cholic acid was obtained, with a content of 99.3%.

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Abstract

The present invention discloses a fine purification method for cholic acid crude product, including the steps as follows: the cholic acid crude product is added with right amount glacial acetic acid water solution to solid phase extract, the acetic acid is recovered from the filtrate after filtering the extraction liquid, and A article is obtained by drying the educt; the A article is added with right amount triethylamine solution to solid phase extract, the pH value of a filtrate after filtrating the extraction liquid is adjusted in a range from 2 to 3 by dilute sulphuric acid, filtering and the educt is washed by water to obtain a B article; the B article and ethanol are mixed with each other to heat, reflux and filter, the filtrate is cooled and placed stilly to recrystallize, then filtering, the crystallinesubstance is dried to obtain the finished product. The cholic acid purity of the invention is high, the fine purification effect is specially good, operation is simple, the method of the invention does not use noxious dissolvent, and the cholic acid is easy of a batch production.

Description

technical field [0001] The invention belongs to the technical field of product purification in fine chemical industry, and in particular relates to a method for refining crude cholic acid. Background technique [0002] Cholic acid is a kind of sterol, which is the most abundant among the four main bile acids in human beings. It was discovered by German scientist Heinrich Otto Wieland and its structure was determined, and thus obtained 1927 Nobel Prize in Chemistry. Cholic acid and chenodeoxycholic acid are the major primary bile acids produced in the liver from cholesterol and combine with glycine or taurine to form glycocholic acid, taurocholic acid, glycochenodeoxycholic acid, and taurodeoxycholic acid , and then secreted into the bile. In bile, they are present as sodium or potassium salts (bile salts). In the colon, cholic acid and chenodeoxycholic acid form secondary cholic acids due to the early dissociation of bacteria and 7α dehydroxylation, that is, deoxycholic a...

Claims

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Application Information

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IPC IPC(8): C07J9/00A61P1/16A61P43/00
Inventor 陆其华
Owner 苏州天绿生物制药有限公司