Chenodeoxycholic acid phenylethylamine salt, preparation method and refining method thereof, and chenodeoxycholic acid preparation method

A technology for chenodeoxycholic acid and phenethylamine salts, which is applied in the preparation of amino compounds, steroids, organic chemistry, etc. Remove bile acid impurities and other problems, and achieve the effect of ammonium salt with white color, high content and good impurity removal effect

Pending Publication Date: 2022-01-11
四川澄华生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since chenodeoxycholic acid and cholic acid both contain carboxyl groups, the carboxyl groups will form salts with the organic amines (tert-butylamine, sec-butylamine) protected in the patent, and the impurity content of cholic acid is relatively high, so it cannot be removed by salt formation. Acid impurities, need additional times of alkaline water washing to remove bile acid impurities, and still cannot obtain high content of chenodeoxycholic acid
The content of the chenodeoxycholic acid product obtained by this invention is about 92%, which can meet the quality requirements of some customers, but cannot meet the needs of customers with high content (about 98%) chenodeoxycholic acid

Method used

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  • Chenodeoxycholic acid phenylethylamine salt, preparation method and refining method thereof, and chenodeoxycholic acid preparation method
  • Chenodeoxycholic acid phenylethylamine salt, preparation method and refining method thereof, and chenodeoxycholic acid preparation method
  • Chenodeoxycholic acid phenylethylamine salt, preparation method and refining method thereof, and chenodeoxycholic acid preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] S1 goose oxygen-oxaglean salt (referred to as CD salt) crude product

[0040] The reaction kettle is added to 200kg (2 times the chilloballine weight), 50 kg of water (0.5 times the weight of the chillion), add the chicken bile cream 100 kg; stir up to 60-65 ° C, stir, and regulate pH to 1 ~ 6, solve material; resetting separation; the aqueous layer 50 kg (0.5 times chollery paste is 0.5 times), stirring at 50-55 ° C for 5 minutes, sedation; buteate Layer, 100 kg of water, stirred for 5 minutes, reset separately, butyl acetate (ie, a goose deoxycholic acid solution) weigh, sampling test, measure CDCA (goose deoxycholic acid referred to as) and CA (gallbladder Acid referred to.

[0041] The butyl acetate layer was added to 17.5 kilograms of A-phenylamine, concentrated from no acetate butyl acetate at 60-90 ° C, and the temperature to 60-65 ° C was adjusted, and about 12.5 kg of A-phenylamine, control pH 8-9, The addition of A-phenylamine was accurate in pH, and the temperature...

Embodiment 2

[0067] S1 goose oxygen-oxaglean salt (referred to as CD salt) crude product

[0068] The reaction kettle was added to 200kg (2 times the chilloconoline weight), 50 kg of water was added (0.5 times the choliobes), and the chicken bold paste was added to 100 kg. The temperature is heated to 60-65 ° C, stirred and regulates the pH to 5.0, the material; the sedation is separated; the aqueous layer is 50 kg (0.5 times the chills of the chilli), and the mixture is stirred at 50-55 ° C for 5 minutes. Static separation. Combined with both acetate layer, 100 kg of water, stirred for 5 minutes, resetting the separation, the acetate layer weighing, sampling the test, the CDCA (Goose deoxycholic acid referred to as) and the CA (Cholic acid abbrevantation) content .

[0069] The butyl acetate layer was added to 12 kg of tert-butlamine, stirred at 50-65 ° C for 1 hour, cooled to 25-30 ° C, continued for 1 hour, centrifugally, washing the filter cake with a acetate, deserted oxychloric tert-buta...

Embodiment 3

[0076] The reaction kettle was added to 200kg (2 times the chilloconoline weight), 50 kg of water was added (0.5 times the choliobes), and the chicken bold paste was added to 100 kg. The temperature is heated to 60-65 ° C, stirred and regulates the pH to 1 to 6, the material; the sedation is separated; the aqueous layer is 50 kg (0.5 times the chills of chilli paste), and stirred in 50-55 ° C. 5 Minutes, resetting liquid. Combined with both a acetate layer, 100 kg of water was extracted, stirred for 5 minutes, resetting the separation, and obtained the butyl acetate layer A.

[0077] Some salt organic base screening experiments are as follows:

[0078] A-phenylamine (R - (+) - A-phenylamine: s - (+) - A-athylamine = 1: 1 hoe body): buteate layer A 60-90 ° C concentrated The butyl acetate is 140 liters, adjusting the temperature to 60-65 ° C, adding A-phenylamine to pH to 9. The incubation was stirred for 20-30 minutes, then cooled to 25-30 ° C, the temperature was 30 ° C, stirring...

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Abstract

The invention discloses a chenodeoxycholic acid phenylethylamine salt, a preparation method and a refining method thereof, and a chenodeoxycholic acid preparation method, relates to the technical field of chenodeoxycholic acid extraction, and aims to solve the problem that a chenodeoxycholic acid product with the content of about 98% required by customers cannot be prepared in the prior art. Alpha-phenylethylamine is added into a chenodeoxycholic acid solution to form salt crystals, and chenodeoxycholic acid phenylethylamine salt is obtained through filtering, wherein the alpha-phenylethylamine is racemate or R-(+)-alpha-phenylethylamine. The method has the advantages that the salifying effect of chenodeoxycholic acid and R-(+)-a-phenylethylamine is the best, the selectivity is highest, the chenodeoxycholic acid impurities are mainly removed from the mother liquor obtained by pulping the chenodeoxycholic acid phenylethylamine salt, the lost chenodeoxycholic acid is minimum, the refining yield is highest, the purity is high, the content is high and is 98% or above, the batch is large, and the method is suitable for industrial large-scale application.

Description

Technical field [0001] The present invention relates to the field of biomedical technology, and more particularly to the field of goose deoxycholic acid extraction technology. Background technique [0002] Goose deoxycholic acid (referred to as: CDCA) has the effect of reducing cholesterol saturation in bile, thereby having better therapeutic effects on gallbladder formation. Goose deoxycholic acid is also an important raw material for chemical synthesis bear to oxychloric acid (3α, 7β-dihydroxy-5-choleanic acid, referred to as UDCA); bear oxychloric acid is the main active ingredient in bear bile bile , Have a clear effect on various diseases such as liver and courage. [0003] Goose deoxychol is mainly extracted or semi-synthesized from animal bile, and the main sources are: 1, chicken, goose; 2, pig bile; 3, duck bile. [0004] Patent No. CN200610046855.3 extracts the industrialization of the uteroidal uloxic acid from the pig bile. The process includes: preparing a gallbospel...

Claims

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Application Information

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IPC IPC(8): C07J9/00C07C209/68C07C209/84C07C211/27
CPCC07J9/005C07C209/68C07C209/84C07C211/27
Inventor 张翔向世明黄清东邓治荣董强袁伟彭捷李建超
Owner 四川澄华生物科技有限公司
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