反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5.8 g (29 mmol) of ethyl quinoline-6-carboxylate was stirred in 80 ml of dichloromethane. 6.2 g of m-chloroperbenzoic acid was added to the obtained mixture under cooling with ice, and they were stirred at room temperature overnight. The mixture was washed with 10% aqueous sodium sulfite solution, saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was evaporated. 70 ml of dichloromethane and 35 ml of phosphoryl chloride were added to the residue, and they were stirred at 50° C. overnight. The solvent was evaporated, and the residue was treated with dichloromethane as the extracting solvent by an ordinary method. After the purification by the silica gel chromatography (ethyl acetate/hexane), the title compound was obtained.
WORKUP
后处理
- temperatureunder cooling with ice, and they
- washThe mixture was washed with 10% aqueous sodium sulfite solution, saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated
- addition70 ml of dichloromethane and 35 ml of phosphoryl chloride were added to the residue, and they
- stirringwere stirred at 50° C. overnight
- customThe solvent was evaporated
- additionthe residue was treated with dichloromethane as the extracting solvent by an ordinary method
- customAfter the purification by the silica gel chromatography (ethyl acetate/hexane)