HRID2164146

反应详情

EQUATION

反应方程式

HRID 2164146 的结构方程式

PROCEDURE

实验过程

The damp 4-acetylbenzenesulfonyl chloride from 50 g. of sodium 4-acetylbenzenesulfonate is added in portions, with stirring, to 500 ml. of cold 40% aqueous methylamine. The mixture is stirred at room temperature for 16 hours, then cooled and the precipitate collected by filtration. The solid (which proved to be the N-methylimine derivative of the ketosulfonamide) is dissolved in 300 ml. of 6% hydrochloric acid and the solution is heated at 80°-90° C. for 30 minutes, then cooled. The resulting precipitate of 4-acetyl-N-methylbenzenesulfonamide is collected by filtration and crystallized from aqueous ethanol; m.p. 107°-109° C.

WORKUP

后处理

  1. stirringThe mixture is stirred at room temperature for 16 hours
  2. temperaturecooled
  3. filtrationthe precipitate collected by filtration
  4. dissolutionis dissolved in 300 ml
  5. temperatureof 6% hydrochloric acid and the solution is heated at 80°-90° C. for 30 minutes
  6. temperaturecooled
  7. filtrationThe resulting precipitate of 4-acetyl-N-methylbenzenesulfonamide is collected by filtration
  8. customcrystallized from aqueous ethanol