HRID477479

反应详情

EQUATION

反应方程式

HRID 477479 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.0 of 2,6-dimethoxybenzoic acid suspended in 200 ml of anhydrous methylene chloride are added with 7.65 ml of triethylamine and then with 3.6 ml of oxalyl chloride. The mixture after being stirred at room temperature for three hours is concentrated under reduced pressure, cooled with ice, added with 10 ml of concentrated ammonia, then stirred for half an hour, then again evaporated under reduced pressure, taken with water and filtered. The solid so obtained, after crystallization from methanol, gives 2,6-dimethoxybenzamide with melting point 208°-209° C.; yield is 54%.

WORKUP

后处理

  1. concentrationis concentrated under reduced pressure
  2. temperaturecooled with ice
  3. additionadded with 10 ml of concentrated ammonia
  4. stirringstirred for half an hour
  5. customagain evaporated under reduced pressure
  6. filtrationfiltered
  7. customThe solid so obtained
  8. customafter crystallization from methanol