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Ursodeoxycholic acid triethylamine salt and preparation method thereof, ursodeoxycholic acid and preparation method thereof

A technology of oxycholic acid triethylamine salt and oxycholic acid triethylamine salt, which is applied in the field of pharmaceutical preparations, can solve the problems of secondary environmental pollution, poor yield of ursodeoxycholic acid triethylamine salt, etc. And the effect of improving quality, reducing production cost, and reducing subsequent processing procedures

Pending Publication Date: 2020-12-22
张翔 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a preparation method of ursodeoxycholic acid triethylamine salt, which is used to solve the problems in the prior art: the yield of ursodeoxycholic acid triethylamine salt is poor, and when the waste liquid is treated in the later stage Technical problems that will cause secondary pollution of the environment

Method used

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  • Ursodeoxycholic acid triethylamine salt and preparation method thereof, ursodeoxycholic acid and preparation method thereof
  • Ursodeoxycholic acid triethylamine salt and preparation method thereof, ursodeoxycholic acid and preparation method thereof
  • Ursodeoxycholic acid triethylamine salt and preparation method thereof, ursodeoxycholic acid and preparation method thereof

Examples

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Embodiment 1

[0032]A preparation method of ursodeoxycholic acid triethylamine salt, comprising the following steps;

[0033]Salt once

[0034]100g crude ursodeoxycholic acid was mixed with 600g acetone, the moisture content of the acetone was 0.09%, the temperature was raised to 40~56°C, stirred for 5 minutes, then 30.0g triethylamine was slowly added dropwise, and after 30 minutes of reaction, reflux Stir for 1h, cool down to 10~25℃, continue the reaction for 0.5h, filter to obtain the first filter cake, wash the first filter cake with 50ml of acetone, wash three times, and dry under vacuum at 80℃ to obtain ursodeoxycholic acid three Ethylamine primary salt;

[0035]Secondary salt formation

[0036]Mix 690g of ursodeoxycholic acid triethylamine primary salt with 3430g of acetone, the moisture content of the acetone is 0.09%, add 92.4g of glacial acetic acid, raise the temperature to 40~56℃, stir for 30 minutes, add 181g of triethylamine, 40 Minutes later, reflux and stir for 1 hour, slowly cool down to 10-...

Embodiment 2

[0038]A preparation method of ursodeoxycholic acid triethylamine salt, comprising the following steps;

[0039]Salt once

[0040]100g of crude ursodeoxycholic acid was mixed with 600g of acetone, the moisture content of the acetone was 0.20%, the temperature was raised to 40~56°C, stirred for 5 minutes, then 30.0g of triethylamine was slowly added dropwise, and after 30 minutes of reaction, reflux Stir for 1h, cool down to 10~25℃, continue the reaction for 0.5h, filter to obtain the first filter cake, wash the first filter cake with 50ml of acetone, wash three times, and dry under vacuum at 80℃ to obtain ursodeoxycholic acid three Ethylamine primary salt;

[0041]Secondary salt formation

[0042]690g ursodeoxycholic acid triethylamine primary salt was mixed with 3430g acetone, the moisture content of the acetone was 0.20%, 92.4g glacial acetic acid was added, the temperature was raised to 40~56℃, stirred for 30 minutes, 181g triethylamine was added, 40 Minutes later, reflux and stir for 1 hour,...

Embodiment 3

[0044]A preparation method of ursodeoxycholic acid triethylamine salt, comprising the following steps;

[0045]Salt once

[0046]100g crude ursodeoxycholic acid was mixed with 600g acetone, the moisture content of the acetone was 0.49%, the temperature was raised to 40~56°C, stirred for 5 minutes, and then 30.0g triethylamine was slowly added dropwise, and after 30 minutes of reaction, reflux Stir for 1h, cool down to 10~25℃, continue the reaction for 0.5h, filter to obtain the first filter cake, wash the first filter cake with 50ml of acetone, wash three times, and dry under vacuum at 80℃ to obtain ursodeoxycholic acid three Ethylamine primary salt;

[0047]Secondary salt formation

[0048]690g ursodeoxycholic acid triethylamine primary salt was mixed with 3430g acetone, the moisture content of the acetone was 0.49%, 92.4g glacial acetic acid was added, the temperature was raised to 40~56℃, stirred for 30 minutes, 181g triethylamine was added, 40 Minutes later, reflux and stir for 1 hour, slow...

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Abstract

The invention discloses a preparation method of ursodesoxycholic acid triethylamine salt, wherein the method comprises the following steps: primary salifying: mixing an ursodesoxycholic acid crude product with acetone with the water content of less than or equal to 0.2%, stirring, heating to 40-56 DEG C, adding triethylamine, reacting for a certain time, slowly cooling to 10-25 DEG C, continuing reacting for a certain time, and filtering to obtain a first filter cake, and washing the first filter cake with acetone to obtain ursodeoxycholic acid triethylamine primary salt; and secondary salifying: mixing the ursodeoxycholic acid triethylamine primary salt with acetone with the water content of less than or equal to 0.2%, adding acid, stirring, heating to 40-56 DEG C, adding triethylamine, reacting for a certain time, slowly cooling to 10-25 DEG C, continuing reacting for a certain time, filtering to obtain a second filter cake, and washing the second filter cake with acetone to obtain the ursodeoxycholic acid triethylamine salt. The preparation method is simple, the yield and the quality of the obtained product are remarkably improved, the working efficiency and the product yield are improved, and the production cost of enterprises can be reduced.

Description

Technical field[0001]The present invention relates to the technical field of pharmaceutical preparations, and specifically refers to a triethylamine salt of ursodeoxycholic acid, a preparation method, and a preparation method of ursodeoxycholic acid.Background technique[0002]Ursodeoxycholic acid is the main component of the precious Chinese medicine bear bile. It can increase the secretion of bile acid, inhibit the synthesis of cholesterol, increase the activity of liver catalase, and reduce the concentration of triacylglycerol in the liver and serum. It has immunomodulatory effects in diseases, so it is used to treat gallstones, cholestatic liver disease, fatty liver, primary biliary cirrhosis, various types of hepatitis, toxic liver disorders, cholecystitis, cholangitis and biliary dyspepsia , Bile reflux gastritis, eye diseases, etc.[0003]In the existing CN201710154482.X, 100g of crude product with 80% ursodeoxycholic acid content was added to 6 times volume of 600ml acetone, 0.5...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00C07C211/05C07C209/68
CPCC07J9/005C07C211/05C07C209/68
Inventor 张翔袁伟向世明黄松彭捷张云辉王洪涛蔡黎民黄清东邓治荣刘金凤
Owner 张翔
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