HRID131642

反应详情

EQUATION

反应方程式

HRID 131642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 128.8 g (0.8 mol) of 1H-indole-2-carboxylic acid, of 159.2 g (0.8 mol) of 4-bromocumene, of 111.6 g (0.808 mol) of potassium carbonate and of 8 g (0.1 mol) of copper oxide in 200 ml of dimethylformamide is stirred at reflux for 24 hours. After cooling, 6 l of water are added to the beige suspension obtained. The suspension is filtered and then the insoluble material is taken up in 1 l of a 5N hydrochloric acid solution. This mixture is extracted with 500 ml of dichloromethane. The organic phase is washed with water, dried over sodium sulfate and then concentrated under reduced pressure. After drying under reduced pressure, 204.4 g of a white solid are obtained, which solid is used as is in the following stage.

WORKUP

后处理

  1. temperatureat reflux for 24 hours
  2. temperatureAfter cooling
  3. customobtained
  4. filtrationThe suspension is filtered
  5. extractionThis mixture is extracted with 500 ml of dichloromethane
  6. washThe organic phase is washed with water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. dry with materialAfter drying under reduced pressure, 204.4 g of a white solid
  10. customare obtained