HRID515305
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
PROCEDURE
实验过程
1,4-Difluoro-2-methyl-5-nitrobenzene (1 g) was dissolved in chlorobenzene (6 mL) and N-bromosuccinimide (1.54 g) added followed by benzoyl peroxide (0.2 g). The reaction mixture was stirred at reflux for 2.5 hours then additional benzoyl peroxide (0.2 g) and N-bromosuccinimide (1.54 g) were added. The reaction was refluxed for 2 hours then was cooled to room temperature, quenched with water and extracted with dichloromethane (3×). The combined organics were dried and concentrated under reduced pressure. The oil obtained was triturated with diethyl ether, filtered and the filtrate concentrated under reduced pressure to yield the title compound (3.21 g).
WORKUP
后处理
- temperatureat reflux for 2.5 hours
- temperatureThe reaction was refluxed for 2 hours
- customquenched with water
- extractionextracted with dichloromethane (3×)
- customThe combined organics were dried
- concentrationconcentrated under reduced pressure
- customThe oil obtained
- customwas triturated with diethyl ether
- filtrationfiltered
- concentrationthe filtrate concentrated under reduced pressure