HRID1058330

反应详情

EQUATION

反应方程式

HRID 1058330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

To a solution of 97.0 g (0.646 mol) o-tolylacetic acid in 1.75 L carbon tetrachloride was added 115.0 g (0.646 mol) N-bromosuccinimide and 3.4 g (0.021 mol) 2,2′-azobisisobutyronitrile. The mixture was heated at reflux under a nitrogen atmosphere for 4 h. After the mixture was cooled to 0-5° C. for 30 min, the solids were removed by filtration and washed with a small portion of carbon tetrachloride. This solid was triturated with water (0.8 L), collected on a filter, and washed with 500 mL of water to give 2-bromomethylphenylacetic acid. The filtrate was concentrated to a volume of 150 ml, and the resulting slurry cooled to 0-5° C. for 30 min. A second batch of product was obtained.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux under a nitrogen atmosphere for 4 h
  3. customthe solids were removed by filtration
  4. washwashed with a small portion of carbon tetrachloride
  5. customThis solid was triturated with water (0.8 L)
  6. customcollected on a filter
  7. washwashed with 500 mL of water