HRID2308749

反应详情

EQUATION

反应方程式

HRID 2308749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

7.57 g (0.04 mol) of 4-(4-methylbenzyl)-piperidine are introduced into 35 ml of ethanol, 9.15 g (0.04 mol) of 2-bromo-4'-hydroxypropiophenone and then 4.24 g (0.04 mol) of sodium carbonate are added and the mixture is heated under reflux for 2 hours. It is then cooled with an ice bath and 200 ml of iced water and 100 ml of toluene are added. The mixture is stirred and left to separate and the organic phase is separated off. The aqueous phase is extracted three times with 100 ml of toluene. The organic phases are combined, washed, dried and then evaporated. This gives 13 g of a pasty oil, which is purified by chromatography on silica using acetone as the eluant. 10 g of a pale oil are collected, which is used as such in the subsequent reduction.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 2 hours
  3. temperatureIt is then cooled with an ice bath
  4. waitleft
  5. customto separate
  6. customthe organic phase is separated off
  7. extractionThe aqueous phase is extracted three times with 100 ml of toluene
  8. washwashed
  9. customdried
  10. customevaporated
  11. customThis gives 13 g of a pasty oil, which is purified by chromatography on silica
  12. custom10 g of a pale oil are collected