HRID1011214

反应详情

EQUATION

反应方程式

HRID 1011214 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

795 mg (3.61 mmol) of 2-methyl-4-(trifluoromethoxy)benzoic acid are heated under reflux with 4 ml (54.8 mmol) of thionyl chloride and one drop of DMF for 30 minutes. After cooling, the reaction solution is introduced slowly dropwise into an ice-cooled concentrated aqueous ammonia solution. The resulting precipitate is collected by suction filtration, taken up in 30 ml of water and stirred at 60° C. for 1 h. The mixture is allowed to cool and the solid is collected by filtration and dried under vacuum. Yield 562 mg (71% of theory).

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationThe resulting precipitate is collected by suction filtration
  3. temperatureto cool
  4. filtrationthe solid is collected by filtration
  5. customdried under vacuum