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ChemicalBook CAS DataBase List Isorhamnetin

Isorhamnetin synthesis

4synthesis methods
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Yield:480-19-3 96.7%

Reaction Conditions:

with potassium hydrogensulfate;sodium hydrogencarbonate;sodium carbonate in dichloromethane;water;acetone at 20; pH=9; for 42 h;

Steps:

1.4; 2.4; 3.4; 4.4; 5.4 example 1

3'--methoxy-4 ', 5,7-- trihydroxy chalcone 10g added 70ml dichloromethane / acetone (V:V = 4:3) mixed solvent. Adding sodium carbonate / bicarbonate buffer solution 100ml (Na2CO34g, NaHCO34g, 100ml water), and stirred vigorously at room temperature and then slowly added dropwise6g potassium hydrogen sulfate complex70ml of an aqueous solution of salts, 5h addition was complete, the reaction at room temperature 16h. Then slowly added dropwise 6g 70ml aqueous solution of potassium hydrogen sulfate complex salt, 5h addition was complete, the reaction was continued at room temperature for 16h. Throughout the course of the reaction, remains reaction system pH = 9. after the reaction was stopped after the disappearance of starting material spot, allowed to stand, the organic phase was separated, the aqueous phase was extracted with methylene chloride, the combined organic phases were washed with saturated sodium thiosulfate and the organic phase was washed with saturated brine 3 times, dried over anhydrous magnesium sulfate, and filtered. the filtrate was added 30mg of p-toluenesulfonic acid, the reaction mixture was stirred at room temperature for 1h, solvent recovery, dry methanol / dichloromethane recrystallized 9.5 g of a pale yellow solid, yield 95

References:

CN105481814,2016,A Location in patent:Paragraph 0020; 0025; 0035; 0040; 0045

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