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
Under an inert atmosphere, 27.5 mmol of boron tribromide/dimethyl sulphide complex are dissolved in 100 ml of dichloromethane and stirred for 15 minutes at ambient temperature. A solution of 13.7 mmol of N-[2-(7-methoxy-1-naphthyl)ethyl]acetamide in 50 ml of dichloromethane is added, and the reaction mixture is heated at reflux for 30 hours. After cooling, the reaction mixture is cautiously hydrolysed and the dichloromethane is evaporated off. The mixture is then extracted with ethyl acetate and the combined organic phases are washed with an aqueous 1M potassium hydrogen carbonate solution. The organic phase is dried over magnesium sulphate and concentrated to yield the title compound. White solid.
WORKUP
后处理
- temperaturethe reaction mixture is heated
- temperatureat reflux for 30 hours
- temperatureAfter cooling
- customthe dichloromethane is evaporated off
- extractionThe mixture is then extracted with ethyl acetate
- washthe combined organic phases are washed with an aqueous 1M potassium hydrogen carbonate solution
- dry with materialThe organic phase is dried over magnesium sulphate
- concentrationconcentrated