HRID29920
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
7-Methoxy-4-phenyl-2H-phthalazin-1-one (740 mg, 2.9 mmol) is dissolved in 7 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 200 mL of water with stirring. The mixture is then stirred at 5° C., basified with 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, 750 mg of product are obtained in the form of a beige-coloured powder.
WORKUP
后处理
- temperatureThe reaction medium is cooled to room temperature
- stirringThe mixture is then stirred at 5° C.
- extractionextracted with dichloromethane
- washThe organic phase is washed with water
- dry with materialwith brine and dried over anhydrous sodium sulfate
- filtrationAfter filtration and evaporation under reduced pressure, 750 mg of product
- customare obtained in the form of a beige-coloured powder