HRID426179

反应详情

EQUATION

反应方程式

HRID 426179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 3,5-dimethylbromobenzene (80.25 g, 0.43M), NBS (77 g, 0.43M), and benzoyl peroxide (5.2 g, 0.021M) in carbon tetrachloride (400 ml) was refluxed for 3 hr. under a light of 500 W tungsten light. After cooling to room temperature, the mixture was filtered and the filtrate was evaporated in vacuo to give a white solid, which was purified by silica gel column chromatography (eluent, hexane) to afford 82 g (72%) of a white solid. m.p. 46-47° C.; 1H NMR (200 MHz, CDCl3) δ 2.32 (3H, s), 4.38 (2H, s), 7.12 (1H, s), 7.25 (1H, s), 7.33 (1H, s).

WORKUP

后处理

  1. temperaturewas refluxed for 3 hr
  2. filtrationthe mixture was filtered
  3. customthe filtrate was evaporated in vacuo
  4. customto give a white solid, which
  5. customwas purified by silica gel column chromatography (eluent, hexane)