HRID515305

反应详情

EQUATION

反应方程式

HRID 515305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureat reflux for 2.5 hours
  2. temperatureThe reaction was refluxed for 2 hours
  3. customquenched with water
  4. extractionextracted with dichloromethane (3×)
  5. customThe combined organics were dried
  6. concentrationconcentrated under reduced pressure
  7. customThe oil obtained
  8. customwas triturated with diethyl ether
  9. filtrationfiltered
  10. concentrationthe filtrate concentrated under reduced pressure