HRID251516

反应详情

EQUATION

反应方程式

HRID 251516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Aluminium trichloride (210.2 g) was added to 1,2-difluorobenzene (200.0 g) at room temperature. The obtained slurry was heated to 50° C., then chloroacetyl chloride (198.0 g) was added over 50 minutes. The reaction mixture was stirred for an additional 60 minutes, then added slowly to a mixture of ice (786.0 g), water (196.0 g) and 37 wt % hydrochloric acid (297.0 g), during the addition the temperature was kept below 60° C. After the addition, the reaction mixture was heated to 60° C. and the layers separated. The organic layer was washed twice with a 20 w/v % sodium chloride solution (200.0 mL). 2-Chloro-1-(3,4-difluorophenyl)ethanone (270.2 g) was obtained by vacuum distillation of the organic layer.

WORKUP

后处理

  1. customwas kept below 60° C
  2. additionAfter the addition
  3. temperaturethe reaction mixture was heated to 60° C.
  4. customthe layers separated
  5. washThe organic layer was washed twice with a 20 w/v % sodium chloride solution (200.0 mL)