HRID1761006

反应详情

EQUATION

反应方程式

HRID 1761006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

A mixture of 4-methoxy-2-methyl-benzoic acid methyl ester (20 g, 111 mmol), N-bromosuccinimide (20.7 g, 117 mmol) and dibenzoylperoxide (0.54 g, 2 mmol) in CCl4 (150 mL) was irradiated with a 300 W lamp. The reaction maintains a steady reflux and after 4.5 h, the lamp was removed and the mixture cooled to 5° C. The mixture was then filtered, the filtrate evaporated and the residue purified twice by chromatography (SiO2, Heptane:Diethyl ether: 95:5 to 85:15) to afford the title product (16.6 g, 58%) as a white solid. MS m/e=258.1 (M−H+).

WORKUP

后处理

  1. customwas irradiated with a 300 W lamp
  2. temperaturea steady reflux and after 4.5 h
  3. customthe lamp was removed
  4. filtrationThe mixture was then filtered
  5. customthe filtrate evaporated
  6. customthe residue purified twice by chromatography (SiO2, Heptane:Diethyl ether: 95:5 to 85:15)