HRID1087177

反应详情

EQUATION

反应方程式

HRID 1087177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(2,4-difluorophenylthio)-4-nitrobenzoyl chloride (1.2 g) in ether (8 ml) was added to a stirred mixture of 40% methylamine (2 ml), water (8 ml) and ether (5 ml) at 0° to 5° C. The mixture was stirred at the same temperature for 1 hour and at room temperature for 1 hour. The organic layer was separated, washed with water, dried and concentrated. The oily residue was crystallized from a mixture of ethyl acetate and hexane to give crystals of N-methyl-3-(2,4-difluorophenylthio)-4-nitrobenzamide (0.7 g).

WORKUP

后处理

  1. customThe organic layer was separated
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe oily residue was crystallized from a mixture of ethyl acetate and hexane