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Method for preparing enoxolone

A technology of glycyrrhetinic acid and glycyrrhizic acid, applied in the direction of steroids, organic chemistry, etc., can solve the problems of difficult industrialization of preparation conditions and process technology, and achieve good separation and purification effect

Inactive Publication Date: 2005-01-12
NANKAI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although pure glycyrrhetinic acid can be obtained by enzymatic hydrolysis and chemical purification, the preparation conditions and process technology are not easy to realize industrialization

Method used

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  • Method for preparing enoxolone
  • Method for preparing enoxolone

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Effect test

Embodiment 1

[0016] Take 40g of crude glycyrrhizic acid (content about 40%), heat and dissolve with 400ml of alcohol for 4 hours, filter out insoluble impurities, adjust the pH of the filtrate to 7-8 with concentrated ammonia water, distill and recover the alcohol, dissolve the residue with 300ml of water, and pass the aqueous solution through ADS -10 macroporous adsorption resin columns (50, 50, 50ml) for three-column adsorption in series, rinse the resin column with water, combine the effluent and washing solution, add concentrated hydrochloric acid until the acid concentration of the solution is 3%, and 200ml of alcohol, heat to reflux After 6 hours, place in cold, filter the precipitated solid, wash with water, and dry in the air to obtain crude glycyrrhetinic acid. The saturated resin column is regenerated with ammonia water-ethanol solution, and the resin column can be used for the next-cycle adsorption after washing with water.

[0017] The crude product of glycyrrhetinic acid was f...

Embodiment 2

[0019] 10g monoammonium glycyrrhizinate (content about 70%), add 100ml of water and heat to dissolve, add dropwise 20ml of concentrated hydrochloric acid, add 70ml of ethanol, stir and reflux for 6 hours, cool, filter the precipitated solid, wash with water, and dry the solid , to obtain crude glycyrrhetinic acid. After further purification and recrystallization, 2.3 g of pure glycyrrhetinic acid product can be obtained. Purity 96% (HPLC method).

Embodiment 3

[0021] 100g monopotassium glycyrrhizic acid (content about 80%), after heating and dissolving with 500ml water, add 300ml ethanol, add 100ml concentrated hydrochloric acid dropwise under stirring, reflux reaction for 6 hours, place in cold place, filter the precipitated solid, wash with water, solid The mixture was dissolved in 400ml of chloroform, the insoluble solids were filtered out, extracted twice with 1mol / L NaOH aqueous solution, the aqueous phases were combined, neutralized to pH 2-3 with hydrochloric acid, and the aqueous phase was extracted twice with chloroform. The chloroform phase was washed with water, concentrated, and the residue was recrystallized with ethanol to obtain 22.3 g of a glycyrrhetinic acid product with a purity of 96%. After the second recrystallization, 18.2 g of the product was obtained. Purity ≥ 98%.

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Abstract

The invention discloses a method for preparing glycyrrhetinic acid. It adopts the glycyrrhizic acid crude product as raw material, and utiizes the processes of ethyl alcohol extraction, using ammonia water to regulate pH value, concentrating and recovering ethyl alcohol, adding water to make dissolution, using ADS-10 macroporous adsorption resin to remove impurity component so as to purity the glycyrrhizic acid being in effluent of resin column, the making acid hydrolysis to obtain the glycyrrhetinic acid crude product, making further purification so as to obtain high-purity glycyrrhetinic acid. The advantage of said invention lies in that the glycyrrhizic acid with different purities can be used to prepare glycyrrhetinic acid, the purification of glycyrrhetinic acid has no need of column chromatography, and adopts the method for making respective extraction at twice by using organic solvent.

Description

technical field [0001] The invention relates to a preparation method of glycyrrhetinic acid. Background technique [0002] Licorice is a commonly used traditional Chinese medicine, widely used in medicine, tobacco, food and other fields. Its main active ingredient, glycyrrhizic acid, has corticotropic hormone-like effects and can be used for detoxification, anti-inflammatory, antitussive, and anti-tumor effects. The aglycon of glycyrrhizic acid is glycyrrhetinic acid, which is hydrolyzed by gastric acid or decomposed by β-glucuronidase in the liver to form glycyrrhetinic acid. The pharmacological effects of glycyrrhizic acid are essentially the effects of glycyrrhetinic acid; recent pharmacological research It was found that glycyrrhizic acid and glycyrrhetinic acid drugs have anti-inflammatory, anti-ulcer, anti-allergic, anti-viral, hypolipidemic, antitussive, asthma and expectorant effects, and can also be used to prevent and treat viral hepatitis, hyperlipidemia and canc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 范云鸽史作清施荣富路延龄
Owner NANKAI UNIV
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