HRID1794132

反应详情

EQUATION

反应方程式

HRID 1794132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Bromo-2,4-difluoro-3-methyl-benzene (22 g, 0.106 M) and N-bromosuccinimide (22.7 g, 0.128 M) were dissolved in tetrachloromethane (800 mL). Dibenzoylperoxide (0.52 g, 2 mM) was added and the mixture was irradiated for 1 h. Succinimide was removed by filtration of the cooled mixture and the filtrate was washed with water. The water phase was extracted with dichloromethane. Organic phases were pooled, dried with MgSO4 and and evaporated to yield a yellowish oil (32 g). The residue was purified by column chromatography (silica gel; n-hexane) to yield 28.4 g (94%) of the title compound as a colorless oil. MS (EI): 286.0 (M)+.

WORKUP

后处理

  1. customthe mixture was irradiated for 1 h
  2. customSuccinimide was removed by filtration of the cooled mixture
  3. washthe filtrate was washed with water
  4. extractionThe water phase was extracted with dichloromethane
  5. dry with materialdried with MgSO4
  6. customevaporated