HRID2094774

反应详情

EQUATION

反应方程式

HRID 2094774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The clear solution of 3-trifluoromethyl-4-chloroaniline (35 g, 0.1789 mol) and pyridine (36 ml, 0.447 mol) in dichloromethane (350 ml) was cooled at 0° C. to −5° C. and a solution of trichloro acetyl chloride (26 ml, 0.2326 mol) in dichloromethane (75 ml) was added drop wise maintaining temperature of the reaction mass below 0° C. The reaction mass was stirred for 1 hour below 0° C. and quenched with water (150 ml) below 5° C. The organic phase was separated and aqueous layer was reextracted with dichloromethane. The combined dichloromethane layer was then washed with water, dried over sodium sulfate and evaporated under vacuum to obtain (55 g) the desired product, i.e., 2,2,2-trichloro-N-(4-chloro-3-(trifluoromethyl)phenyl)acetamide.

WORKUP

后处理

  1. temperaturewise maintaining temperature of the reaction mass below 0° C
  2. customquenched with water (150 ml) below 5° C
  3. customThe organic phase was separated
  4. washThe combined dichloromethane layer was then washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under vacuum