HRID427513

反应详情

EQUATION

反应方程式

HRID 427513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-bromo-o-xylene (15 g, 81 mmol), N-bromo succinimid (15.1 g, 85.1 mmol), dibenzoylperoxid (0.65 g) and tetrachloromethane (150 ml) was refluxed for 5 hours. After filtration the filtrate was washed with sodium hydrogensulfite and water. The organic layer was dried over sodium sulfate and evaporated in vacuo. Chromatography (SiO2) (petroleum ether:ethyl acetate, 100:4) gave a 16.8 g fraction of a mixture containing 45% of the title compound. This mixture was used without further purification.

WORKUP

后处理

  1. temperaturewas refluxed for 5 hours
  2. filtrationAfter filtration the filtrate
  3. washwas washed with sodium hydrogensulfite and water
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customevaporated in vacuo
  6. customChromatography (SiO2) (petroleum ether:ethyl acetate, 100:4) gave a 16.8 g fraction of a mixture