HRID15253

反应详情

EQUATION

反应方程式

HRID 15253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

23.7 g of acrylamide and 60 ml of triethylamine were dissolved in 100 ml of dichloromethane in a flask. To the solution was then added dropwise 27.6 g of acetyl chloride at a temperature of −30° C. After the termination of the dropwise addition, the mixture was then stirred at a temperature of 0° C. for 10 hours. Triethylamine hydrochloride thus precipitated was then filtered off. The filtrate was then subjected to distillation under reduced pressure to remove the solvent therefrom. The residue thus obtained was then subjected to column chromatography with ethyl acetate as a developing solvent and silica gel as a filler to obtain 1.5 g of the desired compound (yield: 4%).

WORKUP

后处理

  1. additionAfter the termination of the dropwise addition
  2. customTriethylamine hydrochloride thus precipitated
  3. filtrationwas then filtered off
  4. distillationThe filtrate was then subjected to distillation under reduced pressure
  5. customto remove the solvent
  6. customThe residue thus obtained