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Method for preparing glycyrrhetinic acid through dual phase hydrolysis method
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A technology of glycyrrhetic acid and hydrolysis method, applied in the direction of steroids, organic chemistry, etc., can solve the problem of no promotion of cell necrosis
Inactive Publication Date: 2015-08-26
李玉山
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Wu Xiaoling et al. reported that 18β-glycyrrhetinic acid inhibited U937 cell proliferation and Induces its apoptosis and does not promote cellnecrosis
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[0040] Pump 500kg of purified water into the reaction kettle, add 15kg of concentrated sulfuric acid under stirring, add 1.0-1.5% antioxidantsodiumsulfite, add 500kg of toluene, slowly add 100.0kg of glycyrrhizinic acid, seal the reaction kettle mouth, heat, wait for the pressure gauge on the reaction kettle When the indicated pressure reaches 0.10Mpa, close the heat-carrying steam valve, and start timing when the pressure rises to 0.15Mpa, keep the pressure in the kettle at 0.12-0.15Mpa, and react for 1-3h. The reaction was detected by thin-layer chromatography. After the reaction was complete, the pressure was lowered, and the interlayer of the reaction kettle was cooled by running tap water under full agitation. It was left to stand for 24 hours, and the layers were separated. The toluene phase was collected, and the water liquid was discarded. Concentrate the toluene solution to dryness at -(0.090-0.095)Mpa, add 350kg ethanol to the concentrate to dissolve, add 3-5% activ...
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Abstract
The invention relates to a method for preparing glycyrrhetinic acid through a dual phase hydrolysis method. The method comprises: 1) dual phase hydrolysissystem preparation; 2) glycyrrhizic acid hydrolysis; 3) hydrolyzate layering, separation, and concentration; 4) glycyrrhetinic acid dissolution, decolorization, concentration and crystallization; and 5) drying and crushing. According to the present invention, the glycyrrhizic acid is adopted as the raw material, the dual phase hydrolysis method is used to prepare the glycyrrhetinic acid, the organic phase is added to the acid hydrolyzate, and the aglycon is transferred into the organic phase when the aglycon is produced during the reaction process so as to avoid the further contact of the aglycon and the acid and avoid the damage on the aglycon in the strong acid environment; and the acid water is added with benzene, toluene, chloroform, dichloromethane or n-butanol to prepare the dual phase system, such that the generated glycyrrhetinic acid is transferred into the organic phase and is separated from the acid so as to accelerate the glycyrrhizic acid hydrolysis rate and improve the yield and the quality of the glycyrrhizic acid hydrolysis.
Description
technical field [0001] The invention relates to a method for preparing glycyrrhetinic acid by a two-phase hydrolysis method. Background technique [0002] Glycyrrhetinic acid (Glycyrrhetinic acid) molecular formula: C 30 h 46 o 4 , Molecular weight: 470.68384, CAS NO.471-53-4, MDL NO.MFCD00003706, EINECS NO.207-444-6, RTECS NO.RK0180000, BRN NO.2229654. beta-glycyrrhetinic acid; (3B,20B)-3-hydroxy-11-oxo-olean-12-ene-29-oic acid; (3β,20β)-3-hydroxy-11-oxo-oleanic acid fruc-12-ene-29-oic acid; 3β-hydroxy-11-oxo-12-oleanene-30-oic acid; glycyrrhetinic acid; 18 BETA-glycyrrhetinic acid; BETA-glycyrrhetinic acid; English aliases: (2S, 4AS, 6AS, 6BR, 8AR, 10S, 12AS, 12BR, 14BR)-10-Hydroxy-2, 4A, 6A, 6B, 9, 9, 12A-Heptamethyl-13-oxo-1, 2 , 3, 4, 4A, 5, 6, 6A, 6B, 7, 8, 8A, 9, 10, 11, 12, 12A, 12B, 13, 14B-Icosa hydro-Picene-2-Carboxylic; acid; (3beta , 18alpha, 20beta)-3-Hydroxy-11-oxoolean-12-en-29-oic acid; 3beta-Hydroxy3-beta-Hydroxy-11-oxo-18beta, 20beta-olean-12-en-29-o...
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