HRID616028

反应详情

EQUATION

反应方程式

HRID 616028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A mixture of 8 g of 3-(3',4'-dimethoxyphenyl)-piperidine, 80 ml of benzene and 3.6 ml of acetic acid anhydride was stirred at 20° C for an hour and was then diluted with 100 ml of water. 500 ml of an aqueous solution saturated with sodium bicarbonate were added thereto and the mixture was stirred for an hour and then was decanted. The aqueous phase was re-extracted with ethyl acetate and the organic phases were washed with water, dried and evaporated to dryness. The residue was chromatographed over silica gel and was eluted with a 6-3-1 cyclohexane-chloroform-triethylamine mixture to obtain 6.75 g of N-acetyl-3-(3',4'-dimethoxyphenyl)-piperidine.

WORKUP

后处理

  1. stirringthe mixture was stirred for an hour
  2. customwas decanted
  3. extractionThe aqueous phase was re-extracted with ethyl acetate
  4. washthe organic phases were washed with water
  5. customdried
  6. customevaporated to dryness
  7. customThe residue was chromatographed over silica gel
  8. washwas eluted with a 6-3-1 cyclohexane-chloroform-triethylamine mixture