HRID382318

反应详情

EQUATION

反应方程式

HRID 382318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under an inert atmosphere, 27.5 mmol of the boron tribromide/dimethyl sulphide complex are dissolved in 100 ml of dichloromethane and stirred for 15 minutes at room 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 refluxed for 30 hours. After cooling, the reaction mixture is hydrolysed cautiously and the dichloromethane is removed by evaporation. 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

  1. temperaturethe reaction mixture is refluxed for 30 hours
  2. temperatureAfter cooling
  3. customthe dichloromethane is removed by evaporation
  4. extractionThe mixture is then extracted with ethyl acetate
  5. washthe combined organic phases are washed with an aqueous 1M potassium hydrogen carbonate solution
  6. dry with materialThe organic phase is dried over magnesium sulphate
  7. concentrationconcentrated