HRID903187

反应详情

EQUATION

反应方程式

HRID 903187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 200 g. of 2-fluorobiphenyl in 1500 ml. of CS2 was cooled to 0°-5° C. and treated with 200 g. of aluminum chloride over 140 minutes and then with 113 g. of acetyl chloride over 165 minutes. The mixture was allowed to warm to room temperature and stirred overnight. The reaction mixture was then poured carefully into ice and hydrochloric acid, and organic material was extracted with a mixture of diethyl ether and ethyl acetate. The organic extract was washed with water, 10% sodium hydroxide, and water, and dried over sodium sulfate. Evaporation of the solvents in vacuo and recrystallization of the solid residue from hexane gave (4'-(2-fluorophenyl)acetophenone. This was recrystallized from hexane to give two crops.

WORKUP

后处理

  1. additiontreated with 200 g
  2. extractionwas extracted with a mixture of diethyl ether and ethyl acetate
  3. extractionThe organic extract
  4. washwas washed with water, 10% sodium hydroxide, and water
  5. dry with materialdried over sodium sulfate
  6. customEvaporation of the solvents
  7. customin vacuo and recrystallization of the solid residue from hexane