Method for preparing cycloastragenol by degrading astragaloside
A technology of astragaloside IV and cycloastragenol, which is applied in the field of medicine and chemical industry, can solve the problems of cumbersome steps, difficult control of reaction conditions, and many preparation steps, and achieve the effects of avoiding excessive reaction, improving stability, and simple steps
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Embodiment 1
[0029] In a mixed medium of 150 mL methanol and 150 mL tetrahydrofuran, 1 g of astragaloside IV with a purity of 98% and 25 g of sodium bisulfate were added, and the reaction was stirred in a water bath at 60°C for 20 hours, cooled and filtered, and the obtained filtrate was neutralized with a dilute alkaline solution, The organic solvent was removed by rotary evaporation, and water was added to 100 mL, and then extracted three times with an equal volume of ethyl acetate. The ethyl acetate was combined and dried over anhydrous sodium sulfate. The ethyl acetate was removed by rotary evaporation to obtain the crude cycloastragalus alcohol. 100-200 mesh silica gel was used as the stationary phase, and 19:1 dichloromethane-methanol mixture was used as the mobile phase for column chromatography purification to obtain 0.33 g of cycloastragalus alcohol with a yield of 52.7% and a purity of 97.5%.
Embodiment 2
[0031] In a mixed medium of 50 mL of ethylene glycol and 200 mL of ethyl acetate, 1 g of astragaloside IV with a purity of 85% and 20 g of potassium hydrogen sulfate were added, and the reaction was stirred for 12 hours in a 90° C. water bath, cooled, and filtered. The obtained filtrate was neutralized with dilute alkali solution, and then 50 mL of distilled water was added, and separated with a separatory funnel. The aqueous phase was extracted three times with 100 mL of ethyl acetate, and the ethyl acetate was combined and dried over anhydrous sodium sulfate. The ethyl acetate was removed by rotary evaporation to obtain the crude cycloastragalus alcohol. Then, 100-200 mesh silica gel was used as the stationary phase, and a 19:1 dichloromethane-methanol mixture was used as the mobile phase for column chromatography purification to obtain 0.28 g of cycloastragalus alcohol with a yield of 50.5% and a purity of 95.6%.
Embodiment 3
[0033] In a mixed medium of 150 mL of absolute ethanol and 150 mL of dioxane, 1 g of astragaloside IV with a purity of 98% and 20 g of ammonium hydrogen sulfate were added, and the reaction was stirred in a water bath at 80°C for 16 hours, cooled and filtered to obtain a dilute filtrate. The alkali solution was neutralized, the organic solvent was removed by rotary evaporation, and water was added to 150 mL, then extracted three times with an equal volume of ethyl acetate, the ethyl acetate was combined, and dried over anhydrous sodium sulfate. The ethyl acetate was removed by rotary evaporation to obtain the crude cycloastragalus alcohol. Then, 100-200 mesh silica gel was used as the stationary phase, and 19:1 dichloromethane-methanol mixture was used as the mobile phase for column chromatography purification to obtain 0.34 g of cycloastragalus alcohol with a yield of 54.9% and a purity of 98.5%.
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