HRID1980805

反应详情

EQUATION

反应方程式

HRID 1980805 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Anhydrous aluminium chloride (66 g) was added to a solution of N,N-dimethylphenethylamine (22.358 g) in dried carbon disulfide (225 ml). Then, propionyl chloride (15.27 g) was added dropwise to the solution at 50° to 60° C. with stirring over a period of about 1 hour and the solution was refluxed with stirring for 4.5 hours. Cold water was added to the solution to decompose the aluminium chloride. The solution was adjusted to weak alkaline with sodium hydroxide solution and extracted with ethyl ether. The ethereal extract was dried over anhydrous sodium sulfate, concentrated and distilled under reduced pressure to give p-N,N-dimethylaminoethylpropiophenone (25 g, 81%) as a fraction boiling at 115°-117° C./1-2 mmHg.

WORKUP

后处理

  1. temperaturethe solution was refluxed
  2. stirringwith stirring for 4.5 hours
  3. extractionextracted with ethyl ether
  4. extractionThe ethereal extract
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. distillationdistilled under reduced pressure