HRID1769563

反应详情

EQUATION

反应方程式

HRID 1769563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A reaction vessel was charged with 113 g of anhydrous aluminum chloride and 600 ml of methylene chloride. To the mixture was added dropwise 113 g of acetyl chloride with stirring at a temperature not higher than 0° C., and was then added dropwise a solution of 100 g of 4-bromo-2-fluoro-biphenyl in 400 ml of methylene chloride. The mixture was reacted with stirring for 7 hours while gradually bringing it back to room temperature. The reaction liquid was poured into ice and diluted hydrochloric acid. The methylene chloride layer was washed successively with water, an aqueous solution of sodium hydrogen carbonate and water, and then dried over Glauber's salt. The solvent was then distilled off and the residue was recrystallized from acetone to give 96 g (82.2%) of 4-acetyl-2'-fluoro-4'-bromobiphenyl.

WORKUP

后处理

  1. customThe mixture was reacted
  2. stirringwith stirring for 7 hours
  3. customback to room temperature
  4. customThe reaction liquid
  5. washThe methylene chloride layer was washed successively with water
  6. dry with materialan aqueous solution of sodium hydrogen carbonate and water, and then dried over Glauber's salt
  7. distillationThe solvent was then distilled off
  8. customthe residue was recrystallized from acetone