HRID463681

反应详情

EQUATION

反应方程式

HRID 463681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a three-neck flask equipped with mechanical stirrer, cooled in ice bath under nitrogen atmosphere, place a solution of 4.67 g (0.02 mole) of 4-[(methylsulfonyl)amino]benzoyl chloride in 30 ml of anhydrous THF. Add dropwise a solution of 1.77 g (0.02 mole) of N,N-dimethylethylenediamine in 10 ml of anhydrous THF; white solid precipitate forms immediately. Stir the mixture at ice temperature for one-half hour and at room temperature for one-half hour. Collect the solid by filtration, wash with dichloromethane, and recrystallize from methanol ether mixture to provide the title compound.

WORKUP

后处理

  1. customIn a three-neck flask equipped with mechanical stirrer
  2. temperaturecooled in ice bath under nitrogen atmosphere
  3. waitat room temperature for one-half hour
  4. customCollect the solid
  5. filtrationby filtration
  6. washwash with dichloromethane
  7. customrecrystallize from methanol ether mixture