HRID1883630

反应详情

EQUATION

反应方程式

HRID 1883630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.90 g (19.2 mmol) of 4-chloro-3-methylbiphenyl was dissolved in 100 ml of carbon tetrachloride and to this solution was added 632 mg (3.85 mmol) of 2,2′-azobisisobutylonitrile, and the mixture was stirred at room temperature for 15 minutes. To this solution was added 3.43 g (19.2 mmol) of N-bromosuccinimide, and the mixture was stirred for 3.5 hours while heating under reflux. To the reaction solution was further added 632 mg (3.85 mmol) of 2,2′-azobisisobutyronitrile and 300 mg (1.69 mmol) of N-bromosuccinimide, and the mixture was stirred for 2 hours under reflux with heating. The reaction mixture was filtrated, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography (eluant: hexane) to obtain 4.69 g of 2-chloro-5-phenylbenzyl bromide in the form of colorless transparent oil.

WORKUP

后处理

  1. stirringthe mixture was stirred for 3.5 hours
  2. temperaturewhile heating
  3. temperatureunder reflux
  4. stirringthe mixture was stirred for 2 hours
  5. temperatureunder reflux
  6. temperaturewith heating
  7. filtrationThe reaction mixture was filtrated
  8. concentrationthe filtrate was concentrated