HRID2425108

反应详情

EQUATION

反应方程式

HRID 2425108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Bromosuccinimide (4.67 g, 26.23 mmol) was added to a stirred solution of 6-methyl-2-chloro-1-nitrobenzene (4.5 g, 26.23 mmol) in distilled carbon-tetrachloride. Benzoyl peroxide (0.01 g) was added to the reaction mixture and the mixture was refluxed for 8 h. The solid separated was filtered. The filtrate was concentrated to get the crude product, which was purified by using column chromatography (silica gel, pet.ether 60-80° C.) to obtain the title compound. Yield: 2.69 g, (41%); MS: m/e (Cl) 253 (M+1).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 8 h
  2. customThe solid separated
  3. filtrationwas filtered
  4. concentrationThe filtrate was concentrated
  5. customto get the crude product, which
  6. customwas purified
  7. customcolumn chromatography (silica gel, pet.ether 60-80° C.)