HRID1602400

反应详情

EQUATION

反应方程式

HRID 1602400 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5-fluoro-4-methylbenzofuran and 5-fluoro-6-methylbenzofuran (14.95 g), N-bromosuccinimide (16.57 g), benzoyl peroxide (0.32 g) and carbon tetrachloride (375 ml) was heated under reflux under the illumination of an 80 W flood lamp for 20 h. The mixture was cooled, and filtered and the filtrate evaporated to dryness to give the crude product as an oil (24.0 g). This material was combined with a similar crude product (6.94 g) from an identical reaction run on a smaller scale and purified by chromatography on silica (900 g) using an ether hexane mixture (1:30) as eluant to give the title compound (13.5 g) as an oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux under the illumination of an 80 W flood lamp for 20 h
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. customthe filtrate evaporated to dryness
  6. customto give the crude product as an oil (24.0 g)
  7. custompurified by chromatography on silica (900 g)