HRID591812

反应详情

EQUATION

反应方程式

HRID 591812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Methyl-2-nitrobenzoic acid methyl ester (27.1 g, 138.8 mmol) was dissolved in carbon tetrachloride (500 mL), and N-bromosuccinimide (29.6 g, 166.6 mmol) was added, followed by benzoyl peroxide (6.72 g, 27.7 mmol). The mixture was illuminated and gently refluxed for 4 hours. Then, the mixture was cooled and concentrated, then purified by column chromatography silica gel 230-400 mesh; 10% ethyl acetate in hexanes as eluent) to give 5-bromomethyl-2-nitrobenzoic acid methyl ester. Yield: 17.9 g (47%).

WORKUP

后处理

  1. customThe mixture was illuminated
  2. temperaturegently refluxed for 4 hours
  3. temperatureThen, the mixture was cooled
  4. concentrationconcentrated
  5. custompurified by column chromatography silica gel 230-400 mesh