Preparation method of ammonium 18alpha,beta-H-glycyrrhetate and hydrate thereof

A technology of triammonium glycyrrhizate and monoammonium glycyrrhizate, applied in the field of 18α, can solve the problems of incomplete separation, residual products, affecting yield and the like

Inactive Publication Date: 2015-08-26
李玉山
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Problems solved by technology

(3) According to the difference in the solubility of 18β-H-glycyrrhizinate and 18α-H-glycyrrhizinate in organic phase and water, a heterogeneous reaction is adopted to separate 18α-H-glycyrrhizinate. The process is simple, but due to Using organic reagents, the separation is not complete, and the product remains in the mother liquor, which affects the yield [12-16]

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  • Preparation method of ammonium 18alpha,beta-H-glycyrrhetate and hydrate thereof
  • Preparation method of ammonium 18alpha,beta-H-glycyrrhetate and hydrate thereof
  • Preparation method of ammonium 18alpha,beta-H-glycyrrhetate and hydrate thereof

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[0044] Refining of glycyrrhizic acid: Add 500g of crude glycyrrhizic acid with a content of 75% to 250mL of ethanol with a volume fraction of 95%, stir and extract at 50-60°C for 2.0h, filter the residue with 200mL of ethanol with a volume fraction of 95% at 50-60°C Stir and extract for 1.5 h, and filter the filter residue with 150 mL of ethanol with a volume fraction of 95% at 50-60° C. for 1.0 h. Combine the extracts, add 0.5% EDTA, add 3-5% (W / W) powdered activated carbon, keep warm at 50-60°C for 30 minutes, filter, concentrate the filtrate under reduced pressure to a relative density of 1.15-1.20, let stand, and crystallize. The crystals were peeled off, moved to a porcelain plate, put into a vacuum desiccator, and dried at a temperature of 40-50° C. to obtain 396 g of 18α, β-H-glycyrrhizic acid mixture, with a content of 98.8%.

[0045] Glycyrrhizic acid configuration transformation: Add 200g of the refined glycyrrhizic acid mixture and 800mL of N,N-dimethylformamide int...

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Abstract

The invention relates to a preparation method of ammonium 18alpha,beta-H-glycyrrhetate and a hydrate thereof. The method selecting 75% crude glycyrrhizic acid as a raw material comprises the following steps: purifying the crude glycyrrhizic acid to obtain purified glycyrrhizic acid with the content of above 98%, converting 18alpha,beta-H-glycyrrhizic acid into 18alpha-H-glycyrrhizic acid, and controlling different pH values of the 18alpha-H-glycyrrhizic acid to generate the following different salts: diammonium 18alpha-H-glycyrrhetate, triammonium 18alpha-H-glycyrrhetate and hydrate thereof, and converting 18beta-H-glycyrrhizic acid to generate monoammonium 18beta-H-glycyrrhetate and hydrate thereof. The method has the advantages of simple operation, mild reaction condition, easy control of the quality, high conversion rate, and suitableness for large scale preparation.

Description

technical field [0001] The invention relates to a preparation method of 18α, β-H-glycyrrhizinate ammonium salt and hydrate thereof. Background technique [0002] Glycyrrhizic acid, also known as glycyrrhizic triterpene saponins and glycyrrhizin, is derived from the roots and rhizomes of the leguminous plant licorice (Glycyrrhiza ur alensis Fisch.), and is the main active ingredient in licorice. -13.06%. It is a glycoside composed of glycyrrhetinic acid and 2 molecules of glucuronic acid. It is an oleanane-type pentacyclic triterpene compound, which is transformed from dammarane cation, and the D ring of dammarane cation undergoes a ring expansion reaction to form a C-18 carbopositive with A-B-C-D rings all six-membered rings ion. The aqueous solution is weakly acidic, the pH of 2% solution is 2.5-3.5, hardly soluble in water and dilute ethanol, easily soluble in hot water, and becomes viscous jelly after cooling. Compound glycyrrhizic acid (SNMC, trade name: Meineng) was...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/00
CPCC07H1/00C07H15/256C07J63/008
Inventor 李玉山
Owner 李玉山
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