Pentaacyl liquiritin, tetraacyl liquiritin, and preparation method of liquiritins
A technology of tetra-acyl licorice and penta-acyl licorice is applied in the field of medicine and achieves the effects of easy separation and purification, simple product composition and good selectivity
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Embodiment 1
[0015] Get 50 grams of Liquiritin with a purity of 83%, add it into a mixed solution containing 11.8 grams of acetic acid, 22.5 mL H2SO4 and 150 mL of toluene, heat to reflux, follow TLC, and the reaction ends in 2.5 hours. The solvent of the reaction mixture was evaporated under reduced pressure, 200 mL of water was added, extracted with ethyl acetate, the organic phase was collected, dried over anhydrous magnesium sulfate, and evaporated to dryness to obtain a crude product of tetraacetylliquiritin. The obtained crude product was recrystallized to obtain 39.41 g of product A with a purity of 98.3%, and the yield was 90%.
[0016]
Embodiment 2
[0018] At room temperature, take 20 grams of 98.7% tetraacetylliquiritin, add 100 mL of pyridine and 9.1 grams of acetic anhydride, stir until the complete conversion of tetraacetylliquiritin, pour the reaction mixture into ice water, precipitate a white product, filter, After washing and drying, a white solid was obtained. After recrystallization, 2.4 g of B2 with a purity of 99.5% was obtained, and the yield was 92%.
[0019]
Embodiment 3
[0021] Get 50 grams of Liquiritin with a purity of 83%, add 17.8 grams of n-butyric acid and 22.5 mL of H2SO4 and 150 mL of toluene in the mixed solution, heat to reflux, TLC point plate tracking, and the reaction is over in 4 hours. The solvent in the reaction mixture was evaporated to dryness, 200 mL of water was added, extracted with ethyl acetate, the organic phase was collected, dried over anhydrous magnesium sulfate, and evaporated to dryness to obtain crude tetra-n-butyryl liquiritin. The obtained crude product was dissolved in 250 mL of pyridine, 13.9 g of benzoyl chloride was added, heated to reflux for 2 hours, the reaction mixture was poured into ice water, filtered, washed and dried to obtain a white solid, recrystallized to obtain the product C56. 4 g yield 73%.
[0022]
PUM
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