HRID1868932
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe resulting mixture was refluxed for 15 hours
- temperatureThe mixture was cooled to room temperature
- filtrationfiltered through a plug of Celite
- washwashed with 10% EtOAc/hexane
- concentrationThe organic was concentrated
- custompurified by column chromatography (0-10% EtOAc/hexane)