HRID276070

反应详情

EQUATION

反应方程式

HRID 276070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8.70 g of 2-fluoro-4′-methylbiphenyl, 8.32 g of N-bromosuccinimide, 0.10 g of 2,2′-azobisisobutylonitrile and 150 ml of carbon tetrachloride was heat-refluxed for 5 hours. The reaction solution was washed with water, and the organic layer was concentrated. The resulting residue was purified through silica-gel column chromatography (eluent: a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl. Further, this compound was crystallized from hexane to give 4.93 g of 2-fluoro-4′-bromomethylbiphenyl.

WORKUP

后处理

  1. temperaturewas heat-refluxed for 5 hours
  2. washThe reaction solution was washed with water
  3. concentrationthe organic layer was concentrated
  4. customThe resulting residue was purified through silica-gel column chromatography (eluent
  5. additiona mixture of hexane and ethyl acetate at a ratio of 9:1)
  6. customto obtain crude 2-fluoro-4′-bromomethylbiphenyl
  7. customFurther, this compound was crystallized from hexane