Method for synthesizing 5,6,4'-trihydroxyflavone-7-O-D-glucuronic acid
A technology of glucuronic acid and trihydroxyflavone, applied in chemical instruments and methods, medical preparations containing active ingredients, sugar derivatives, etc., can solve the problems of long synthetic routes and low yields
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Embodiment 1
[0016] Take 2.68g 3,4,5-triacetoxyphenol and 2.50g p-acetoxycinnamic acid chloride, put into 20mL BF 3 -Et 2 O solution, make it fully dissolved, add 2g 4A molecular sieve, heat under reflux for 15 minutes, stop heating, filter, recrystallize with petroleum ether-ethyl acetate (3:1) to obtain 9-hydroxy-5,6,7,4 '-Tetraacetoxychalcone, a total of 4.15g, the transfer rate of this step was 91%.
[0017] Take 4.56g of 9-hydroxy-5,6,7,4'-tetraacetoxychalcone, 200mg of iodine, dissolve in 25mL of DMSO, reflux for 2 hours, then carefully pour into 200g of crushed ice, filter, precipitate with 20% Na 2 SO 3 Washed and recrystallized with petroleum ether-ethyl acetate (10:1) to obtain 3.95 g of 5,6,7,4'-tetraacetoxyflavone with a transfer rate of 87%.
[0018] Take 4.54g 5,6,7,4'-tetraacetoxyflavone, 5.25g K 2 CO 3 , 0.21g KI, 2.3mL PhCH 2 Cl, placed in 600 mL of dry acetone, heated to reflux at 40-45 °C for 4 hours. After the reaction was completed, the solution was diluted wit...
Embodiment 2
[0023] Purification of target products
[0024]Take 100 g of the complete product, add 1000 mL of pure water, adjust the pH value to 7 with 30% sodium hydroxide solution to completely dissolve, filter, add 8 times acetone to the filtrate at 25 ° C for precipitation, add acetone while stirring , make the precipitation complete, stand for 12 hours, filter, add acetone to wash three times, then move the precipitate to another container, add 6 times the amount of 40% acetone, stir well, add 25% hydrochloric acid to adjust the pH value to 1 ~2, stand for 10 hours, filter with suction, wash with water until neutral, add ethanol to wash once, and dry to obtain refined products. HPLC analysis showed that the content of 5,6,4'-trihydroxyflavone-7-O-D-glucuronic acid in the obtained sample was 99.31%.
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