HRID660557

反应详情

EQUATION

反应方程式

HRID 660557 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-methylbenzoic acid ethyl ester (16.4 g, 99.87 mmol) in CCl4 (100 mL) is added N-bromosuccinimide (17.8 g, 100 mmol) and 2,2′-azobisisobutyronitrile (3.28 g, 19.97 mmol). The resulting mixture is heated at reflux for 2 h. After the mixture is cooled to RT, the solid is filtered off and the filtrate is concentrated and extracted with EtOAc. The EtOAc solution is washed with brine and dried over MgSO4, filtered and concentrated to afford the title compound as a pale yellow oil.

WORKUP

后处理

  1. temperatureThe resulting mixture is heated
  2. temperatureat reflux for 2 h
  3. filtrationthe solid is filtered off
  4. concentrationthe filtrate is concentrated
  5. extractionextracted with EtOAc
  6. washThe EtOAc solution is washed with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated