HRID1087222

反应详情

EQUATION

反应方程式

HRID 1087222 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-ethyl-4-amino-3-(2,4-difluorophenylthio)benzamide (0.84 g) and methanesulfonyl chloride (0.57 g) in pyridine (5 ml) was stirred at room temperature overnight. The reaction mixture was concentrated. The residue was dissolved in ethyl acetate, washed with dilute hydrochloric acid, dried and evaporated. The residue obtained was dissolved in methanol and treated with potassium hydroxide (0.4 g). The solution was concentrated and the residue was dissolved in water. The aqueous solution was acidified with dilute hydrochloric acid and extracted with chloroform. The extract was washed with water, dried, and evaporated. The residual solid was recrystallized from ethanol to give N-ethyl-3-(2,4-difluorophenylthio)-4-(methanesulfonamido)benzamide (0.67 g).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with dilute hydrochloric acid
  4. customdried
  5. customevaporated
  6. customThe residue obtained
  7. concentrationThe solution was concentrated
  8. dissolutionthe residue was dissolved in water
  9. extractionextracted with chloroform
  10. washThe extract was washed with water
  11. customdried
  12. customevaporated
  13. customThe residual solid was recrystallized from ethanol