反应详情

温度

80 °C

19 g (67 mmol) of 7-methoxy-4-(4-methoxyphenyl)-2H-phthalazin-1-one are dissolved in 100 mL of phosphoryl chloride. The solution is heated at 80° C. for 2 hours. The reaction medium is cooled to room temperature and then poured slowly into 500 mL of water at 40-50° C. with stirring. The mixture is then stirred at 5° C., basified by addition of 35% sodium hydroxide solution and then extracted with dichloromethane. The organic phase is washed with water and then with brine and dried over anhydrous sodium sulfate. After filtration and evaporation under reduced pressure, 19.3 g of a beige-coloured powder are obtained (yield=96%).

1. temperatureThe reaction medium is cooled to room temperature
2. stirringThe mixture is then stirred at 5° C.
3. extractionextracted with dichloromethane
4. washThe organic phase is washed with water
5. dry with materialwith brine and dried over anhydrous sodium sulfate
6. filtrationAfter filtration and evaporation under reduced pressure, 19.3 g of a beige-coloured powder
7. customare obtained (yield=96%)