HRID1961696

反应详情

EQUATION

反应方程式

HRID 1961696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-chloro-4-methyl-1-trifluoromethylbenzene 26 (0.20 g, 1 mmol), N-bromosuccinimide (0.17 g, 1 mmol) and benzoyl peroxide (7.4 mg, 0.03 mmol) in carbon tetrachloride (2 mL) was heated to reflux for 2 hours. Another portion of benzoyl peroxide (20 mg, 0.08 mmol) was added. The mixture was heated to reflux for another 0.5 hours. The reaction mixture was further stirred at room temperature for 16 hours. The solid was removed by filtration. The solvent was removed under reduced pressure. The crude product was purified by flash chromatography on silica, using petroleum ether as eluent, to give 0.22 g (80%) of Compound 27.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. temperatureThe mixture was heated
  4. temperatureto reflux for another 0.5 hours
  5. customThe solid was removed by filtration
  6. customThe solvent was removed under reduced pressure
  7. customThe crude product was purified by flash chromatography on silica