HRID564445

反应详情

EQUATION

反应方程式

HRID 564445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-bromo-3,5-dimethylbenzene (25.0 g, 135.0 mmol) in CCl4 (150 mL), 1,3-dibromo-5,5-dimethylimidazolidine-2,4-dione (14.5 g, 54.0 mmol) and dibenzoyl peroxide (BPO) (0.2 g) were added and the mixture was refluxed for 7 h. After the reaction was cooled to room temperature, the precipitate was filtered though Celite, and then the solid was rinsed two times with pentane (50 mL). The combined filtrate was washed with water (50 mL), followed by saturated sodium bicarbonate (50 mL) and sodium thiosulfate (50 mL×2). The organic layer was dried over anhydrous sodium sulfate. Evaporation of the solvent afforded the compound 1-bromo-3-(bromomethyl)-5-methylbenzene (35.6 g, 99%).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 7 h
  2. filtrationthe precipitate was filtered though Celite
  3. washthe solid was rinsed two times with pentane (50 mL)
  4. washThe combined filtrate was washed with water (50 mL)
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customEvaporation of the solvent