HRID79426

反应详情

EQUATION

反应方程式

HRID 79426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Bromosuccinimide (2.17 g, 12.2 mmol) and benzoic peroxyanhydride (0.295 g, 1.22 mmol) were added to a flask containing a solution of 1,3-dimethylpyridin-2(1H)-one (1.50 g, 12.2 mmol) in carbon tetrachloride (250 mL, degassed with flowing N2 for 5 minutes). The mixture was heated at reflux for 3 hours. The reaction mixture was cooled to ambient temperature, filtered through filter paper, and the filtrate was concentrated under vacuum. The residue was suspended in diethyl ether (20 mL), stirred for 15 minutes, and the liquid was decanted. The solids were rinsed with diethyl ether (3×5 mL), then dried under vacuum to give 3-(bromomethyl)-1-methylpyridin-2(1H)-one as a yellow solid (1.1 g).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 3 hours
  3. filtrationfiltered
  4. filtrationthrough filter paper
  5. concentrationthe filtrate was concentrated under vacuum
  6. customthe liquid was decanted
  7. washThe solids were rinsed with diethyl ether (3×5 mL)
  8. customdried under vacuum