HRID2078340

反应详情

EQUATION

反应方程式

HRID 2078340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 1-chloro-3-iodo-2-methylbenzene (11 g, 44 mmol) in 60 mL CCl4 was stirred at 70° C. and treated with 1-bromopyrrolidine-2,5-dione (12 g, 65 mmol) and dibenzoyl peroxide (1.1 g, 4.4 mmol) slowly. The resulting mixture was refluxed for 15 hours. The mixture was cooled to room temperature, filtered through a plug of Celite, and washed with 10% EtOAc/hexane. The organic was concentrated and purified by column chromatography (0-10% EtOAc/hexane) to give 14 g pink solid.

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for 15 hours
  2. temperatureThe mixture was cooled to room temperature
  3. filtrationfiltered through a plug of Celite
  4. washwashed with 10% EtOAc/hexane
  5. concentrationThe organic was concentrated
  6. custompurified by column chromatography (0-10% EtOAc/hexane)