HRID341822

反应详情

EQUATION

反应方程式

HRID 341822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 27.6 g (92.4 mmol) of the 4-chloro-6-methyl-2-(2-nitrophenyl)quinoline obtained in Example 1, 110 ml of chloroform was added. After stirring, 15.6 g (87.8 mmol) of N-bromosuccinimide (NBS) was added thereto. Then, 15 ml of chloroform containing 0.78 g of 2,2'-azobis(2,4-dimethylvaleronitrile) was added dropwise thereto, and the thus-prepared mixture was heated under reflux for 1 hour. After cooling to room temperature, the mixture was poured into 220 ml of water and separated out, and the organic layer was washed with 110 ml of water twice. Next, the washed organic layer was evaporated and dried in an evaporator and recrystallized from toluene to obtain 14.7 g of 4-chloro-6-(bromomethyl)-2-(2-nitrophenyl)quinoline.

WORKUP

后处理

  1. temperaturethe thus-prepared mixture was heated
  2. temperatureunder reflux for 1 hour
  3. customseparated out
  4. washthe organic layer was washed with 110 ml of water twice
  5. customNext, the washed organic layer was evaporated
  6. customdried in an evaporator
  7. customrecrystallized from toluene