HRID477479
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationis concentrated under reduced pressure
- temperaturecooled with ice
- additionadded with 10 ml of concentrated ammonia
- stirringstirred for half an hour
- customagain evaporated under reduced pressure
- filtrationfiltered
- customThe solid so obtained
- customafter crystallization from methanol