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Efficient synthetic method for medicinal high-purity dehydrocholic acid

A technology of dehydrocholic acid and synthesis method, applied in steroids, organic chemistry and other directions, can solve the problems of heavy metal residue safety hazards, chlorine leakage, non-conformance and other problems in products, and achieve uniformity, small batch-to-batch variation, Easy-to-use effects

Inactive Publication Date: 2013-05-01
ZHONGSHAN BAILING BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Method 1 and the U.S. patent both use dichromate as an oxidant and introduce heavy metal chromium. Not only the chromium slag collected after the reaction puts pressure on the environment, but also makes the product have a safety hazard of heavy metal residue, which does not comply with the "People's Republic of China Regulations on Heavy Metal Chromium Residues in Abnormal Toxicity Inspection in Pharmacopoeia
The yield of method 2 is low, and the use of chlorine for oxidation can easily cause the leakage of chlorine
Therefore, the above-mentioned methods all have deficiencies

Method used

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  • Efficient synthetic method for medicinal high-purity dehydrocholic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] In a 250ml three-neck round bottom flask, put 10.0g of cholic acid into it, and under the condition of heating in a water bath at 40°C, add 27.5ml of acetone while stirring slowly to disperse the cholic acid evenly, then slowly add 15ml of 65% concentrated sulfuric acid, it can be seen Bile acid gradually dissolves. After the bile acid is completely dissolved, slowly add 100ml of sodium hypochlorite solution dropwise. After the addition, the reaction was incubated for 6 hours, and samples were taken every hour for TLC detection during the period to monitor the reaction process and finally judge the reaction end point. After the reaction was completed, the feed liquid was placed in a 500ml separatory funnel and allowed to stand for stratification. The lower layer was a brine phase, and the upper layer was an acetone phase. The lower layer was discarded, and 275 ml of purified water was added to the upper layer while stirring, and a large amount of white powdery solids w...

Embodiment 2

[0050] In a 50L reactor, put 3kg of cholic acid into it, and under the condition of controlling the temperature of the circulating water in the jacket at 40°C, pump in 8.3L of acetone while stirring slowly to disperse the cholic acid evenly, and then slowly pump in 65% Concentrated sulfuric acid 4.5L, after the cholic acid is completely dissolved, slowly add 30L sodium hypochlorite solution. After the addition, the reaction was incubated for 6 hours, and samples were taken every hour during the process for TLC detection to monitor the reaction progress and finally judge the reaction end point. After the reaction stopped, the layers were left to stand, the lower layer was discarded, the upper layer was transferred to a 200L reactor, 83L of purified water was added, and a large amount of white powdery solids were precipitated. Filter, wash the filter cake with water until neutral, and dry to obtain about 2.6 kg of dehydrocholic acid crude dry powder. The melting point is 236°C-...

Embodiment 3

[0053] In a 50L reactor, put 3kg of cholic acid into it, and under the condition of controlling the temperature of the circulating water in the jacket at 40°C, pump in 8.3L of acetone while stirring slowly to disperse the cholic acid evenly, and then slowly pump in 65% Concentrated sulfuric acid 4.5L, after the cholic acid is completely dissolved, slowly add 30L sodium hypochlorite solution. After the addition, the reaction was incubated for 6 hours, and samples were taken every hour during the process for TLC detection to monitor the reaction progress and finally judge the reaction end point. After the reaction stopped, the layers were left to stand, the lower layer was discarded, the upper layer was transferred to a 200L reactor, 83L of purified water was added, and a large amount of white powdery solids were precipitated. Filter, wash the filter cake with water until neutral, and dry to obtain about 2.6 kg of dehydrocholic acid crude dry powder. The melting point is 236°C-...

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Abstract

The invention discloses an efficient synthetic method for medicinal high-purity dehydrocholic acid. The method is characterized by comprising the following steps: A, cholic acid is evenly dispersed by using acetone, then concentrated sulfuric acid is added for dissolving; sodium hypochlorite is dripped, after the reaction is finished, water is added for mixing and filtering, and is used for washing until the neutral property is obtained, and then the drying is implemented to obtain a crude redox product; and B, after the acetone is added in the crude product of the step A for dissolving, enough silica gel is added for absorbing acid and cholic acid derivative of the crude product, after the absorption is finished, acetone solution of the dehydrocholic acid is obtained through filtering, the acetone solution is dried by distillation, and is added with sodium hydroxide solution for dissolving, then acetic acid solution is dripped, and is crystallized to separate out a dehydrocholic acid crystal, and then the filtration and the drying are implemented to obtain the finished product. The invention aims to overcome the defects in the prior art, and provides the efficient synthetic method for the medicinal high-purity dehydrocholic acid; and the method has the advantages of simple technique, high product purity, high yield, lower production cost, safety and reliability.

Description

technical field [0001] The invention relates to a high-efficiency synthesis method of medicinal high-purity dehydrocholic acid. Background technique [0002] Diseases of the biliary system refer to the lesions that occur in the channels that transport bile inside and outside the liver. There are many such diseases and they are also relatively common. The biliary tract is the only way to transport bile secreted by liver cells to the intestinal tract. Once a disease occurs in a certain part of the biliary tract, it can lead to poor drainage of bile, which is very harmful to the human body. Some biliary system diseases, such as intrahepatic stones, suppurative cholangitis, tumors, etc., are difficult to treat and can be life-threatening. Among them, cholelithiasis refers to a disease in which stones occur in the gallbladder and bile ducts. The etiology of the disease is mainly summarized as three factors: biliary tract infection, cholestasis, and abnormal changes in bile comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 阮宇峰张和平刘遗松霍延豪梁待亮周海香黄文军刘骅沈惠宾邱国华
Owner ZHONGSHAN BAILING BIOTECHNOLOGY CO LTD
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