HRID704454

反应详情

EQUATION

反应方程式

HRID 704454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

100 ml of an N,N-dimethylformamide solution containing 34.2 g (0.20 mol) of p-toluenesulfonamide, was dropwise added over a period of 60 minutes under cooling with ice to a suspension comprising 19.7 g (0.41 mol) of 50% oily sodium hydride and 60 ml of N,N-dimethylformamide. The reaction solution was stirred at room temperature for 30 minutes at 60° C., and then 300 ml of an N,N-dimethylformamide solution containing 47 g (0.20 mol) of 4,5-bischloromethyl veratrol was dropwise added over a period of 90 minutes at 60° C. The reaction solution was stirred at room temperature for 3 hours, and then poured into 2000 ml of water. The precipitated crystals were collected and washed with water to obtain 60 g (yield: 90.0%) of the above identified compound.

WORKUP

后处理

  1. additionwas dropwise added over a period of 60 minutes
  2. additionwas dropwise added over a period of 90 minutes at 60° C
  3. stirringThe reaction solution was stirred at room temperature for 3 hours
  4. customThe precipitated crystals were collected
  5. washwashed with water
  6. customto obtain 60 g (yield: 90.0%) of the