HRID420864

反应详情

EQUATION

反应方程式

HRID 420864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

Dissolve 16.2 g (0.0889 mol) of 3,4-dimethoxy-6-hydroxybenzaldehyde in 80 ml of DMF. Cool to 10° C. and add in portions 24.6 g (0.178 mol) of potassium carbonate. Allow to return to ambient temperature and stir for 30 minutes. Cool to approximately 10° C. and pour in dropwise 10.1 ml (0.093 mol) of N,N-dimethylsulphamoyl chloride. Allow to return to ambient temperature and stir for 2 h. Pour the reaction mixture into 600 g of water and ice and stir for 1 h at ambient temperature. The precipitate formed is filtered off and washed 3 times with 50 ml of water each time and then dried in vacuo. 21.3 g of title product are obtained.

WORKUP

后处理

  1. customto return to ambient temperature
  2. temperatureCool to approximately 10° C.
  3. customto return to ambient temperature
  4. stirringstir for 2 h
  5. stirringstir for 1 h at ambient temperature
  6. customThe precipitate formed
  7. filtrationis filtered off
  8. washwashed 3 times with 50 ml of water each time
  9. customdried in vacuo