HRID1087210

反应详情

EQUATION

反应方程式

HRID 1087210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-amino-3-(2,4-difluorophenylamino)benzonitrile (1.2 g) and methanesulfonyl chloride (0.45 ml) in pyridine (12 ml) was stirred for 4 hours at room temperature. Pyridine was evaporated and the residue was stirred with an aqueous solution of sodium hydroxide (5%; 40 ml) for 10 minutes. The solution was washed with toluene, acidified to pH 3 with hydrochloric acid, and extracted with ethyl acetate. The extract was washed with water, dried and evaporated to dryness. The residue (1.4 g) was recrystallized from ethanol to give colorless prisms of 4'-cyano-2'-(2,4-difluorophenylamino)methanesulfonanilide (1.2 g).

WORKUP

后处理

  1. customPyridine was evaporated
  2. stirringthe residue was stirred with an aqueous solution of sodium hydroxide (5%; 40 ml) for 10 minutes
  3. washThe solution was washed with toluene
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. customdried
  7. customevaporated to dryness
  8. customThe residue (1.4 g) was recrystallized from ethanol