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Preparation method of acetyl glycyrrhetinic acid

A technology of glycyrrhetinic acid and monoammonium glycyrrhizinate, which is applied in the fields of steroids and organic chemistry, can solve the problems of large organic solvent loss, cumbersome preparation process, and high cost. low cost effect

Pending Publication Date: 2022-05-17
XINJIANG FUWO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has the disadvantages of cumbersome preparation process, high energy consumption, large loss of organic solvent, and high cost of producing acetylglycyrrhetinic acid from glycyrrhizic acid powder.

Method used

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  • Preparation method of acetyl glycyrrhetinic acid
  • Preparation method of acetyl glycyrrhetinic acid
  • Preparation method of acetyl glycyrrhetinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method of acetylglycyrrhetinic acid, prepared by the following steps:

[0035] Get 100kg of the dry product of monoammonium glycyrrhizinate mother liquor, add 450kg of glacial acetic acid with a concentration of 85% and stir to dissolve to obtain a mixed solution, then add 20kg of sulfuric acid to the mixed solution, heat up to 90°C, and react for 1.5h to carry out hydrolysis and acetylation. After the above reaction is completed, feed cooling water to reduce the temperature of the reaction system to 40°C, filter, wash with 100kg of glacial acetic acid with a concentration of 65%, then wash with water to pH 5, and dry at 85°C to obtain acetylglycyrrhetinic acid 10.8 kg.

Embodiment 2

[0037] A preparation method of acetylglycyrrhetinic acid, prepared by the following steps:

[0038] Get 120kg of the dry product of monoammonium glycyrrhizinate mother liquor, add 550kg concentration and be 85% glacial acetic acid and stir and dissolve to obtain a mixed solution, then add 30kg of sulfuric acid in the mixed solution, heat up to 95°C, react for 1.5h to carry out hydrolysis and acetylation reaction, After the above reaction is completed, feed cooling water to reduce the temperature of the reaction system to 40°C, filter, wash with 120kg of glacial acetic acid with a concentration of 65%, then wash with water to pH 5.5, and dry at 85°C to obtain acetylglycyrrhetinic acid 12.24 kg.

Embodiment 3

[0040] A preparation method of acetylglycyrrhetinic acid, prepared by the following steps:

[0041] Get 220kg of the dry product of monoammonium glycyrrhizinate mother liquor, add 1000kg concentration and be 85% glacial acetic acid and stir and dissolve to obtain a mixed solution, then add 60kg of sulfuric acid in the mixed solution, heat up to 98°C, react for 1.5h to carry out hydrolysis and acetylation reaction, After the above reaction is completed, feed cooling water to reduce the temperature of the reaction system to 40°C, filter, wash with 250kg of glacial acetic acid with a concentration of 65%, then wash with water to pH 6, and dry at 85°C to obtain acetylglycyrrhetinic acid 22.5 kg.

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Abstract

The invention provides a preparation method of acetyl glycyrrhetinic acid, and belongs to the technical field of acetyl glycyrrhetinic acid preparation. According to the method, by-products in the production process of mono-ammonium glycyrrhizinate are adopted as raw materials, firstly, a dried mono-ammonium glycyrrhizinate mother liquor product is dissolved with a hydrophilic organic solvent, and then the acetyl glycyrrhetinic acid is obtained through catalytic hydrolysis and acetylation with mineral acid. The preparation method of the acetyl glycyrrhetinic acid provided by the invention has the advantages that the process is simplified, the process is easy to control, the production cost is low, the product is purer, the quality of the glycyrrhetinic acid synthesized by the acetyl glycyrrhetinic acid prepared by the method meets EP standard requirements of EU, and the yield is obviously higher than that of the prior art.

Description

technical field [0001] The invention relates to the technical field of preparation of acetylglycyrrhetinic acid, in particular to a preparation method of acetylglycyrrhetinic acid. Background technique [0002] Licorice is a commonly used traditional Chinese medicine, and its main active ingredient, glycyrrhizic acid, has corticotropic hormone-like effects and can be used for detoxification, anti-inflammation, antitussive, and anti-tumor. The aglycone of glycyrrhizic acid is glycyrrhetinic acid. Studies have found that in the human body, glycyrrhizic acid is hydrolyzed by gastric acid or decomposed by β-glucuronidase in the liver to form glycyrrhetinic acid, and then absorbed into the blood through the small intestine, so it finally exerts its medicinal effect. The effect is essentially the effect of glycyrrhetinic acid. Modern studies have shown that glycyrrhetinic acid is superior to glycyrrhizic acid in anti-inflammatory, anti-ulcer, anti-allergic, anti-viral, hypolipide...

Claims

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Application Information

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IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 陈振鸿安晨光王耀红
Owner XINJIANG FUWO PHARMA
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