反应详情

温度

90 °C

1 kg of 3′,5,7-trihydroxy-4′-methoxy flavone-7-rutinoside and 454 g of potassium carbonate were dissolved in dimethylformamide at 10° C., which was heated and stirred at 90° C. for 8 hours. The reaction solution was cooled to room temperature. To the solution was added 1 kg of iodomethane, followed by stirring at room temperature for 12 hours. Upon completing the reaction, 50 L of mixed solution of ethyl acetate and dichloromethane (3:2) was added thereto. The resultant solution was stirred for 30 minutes and then filtered. 5.2 L of methanol and 5 kg of conc. hydrochloric acid were added to the filtered solid, followed by heating to reflux at 65° C. for 8 hours. The reaction mixture was cooled down to room temperature. The precipitated solid were collected by filtration and washed with a small amount of methanol to give a desired compound (yellow solid, 426 g, yield: 82%).

1. temperaturewhich was heated
2. temperatureThe reaction solution was cooled to room temperature
3. stirringby stirring at room temperature for 12 hours
4. additionwas added
5. filtrationfiltered
6. addition5.2 L of methanol and 5 kg of conc. hydrochloric acid were added to the filtered solid
7. temperatureby heating
8. temperatureto reflux at 65° C. for 8 hours
9. temperatureThe reaction mixture was cooled down to room temperature
10. filtrationThe precipitated solid were collected by filtration
11. washwashed with a small amount of methanol