HRID2353371

反应详情

EQUATION

反应方程式

HRID 2353371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-chloro-5-methyl-2-(2-trifluoromethyl-biphenyl-4-yl)-benzo[b]thiophene (110 mg, 0.273 mmol) in CCl4 (3 ml) is added NBS (49 mg, 1 eq.). The mixture is heated at reflux for 15 minutes before AIBN (4.5 mg, 0.1 eq.) is added. The reaction is further heated at reflux overnight. The mixture is filtered through Celite and washed with CCl4. The filtrate is concentrated and purified by column chromatography (EtOAc/Hexane, gradient) to give 50 mg of 5-bromomethyl-3-chloro-2-(2-trifluoromethyl-biphenyl-4-yl)-benzo[b]thiophene in 38% yield.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. additionis added
  3. temperatureThe reaction is further heated
  4. temperatureat reflux overnight
  5. filtrationThe mixture is filtered through Celite
  6. washwashed with CCl4
  7. concentrationThe filtrate is concentrated
  8. custompurified by column chromatography (EtOAc/Hexane, gradient)