HRID22299

反应详情

EQUATION

反应方程式

HRID 22299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.0 g (83.8 mmol) of 2,3-dichloro-thiophenol are introduced into 50 ml of absolute methanol, 4.5 g (83.8 mmol) of sodium methanolate are added in portions, with cooling, and the mixture is stirred for 15 minutes at room temperature. 6.3 g (83.8 mmol) of chloroacetonitrile are subsequently added dropwise, and the mixture is stirred for 2 hours at room temperature and for a further 5 hours at reflux temperature. The entire batch is then filtered while hot and concentrated in vacuo. 10.8 g (59.1% of theory) of 2,3-dichloro-phenylthioacetonitrile are obtained.

WORKUP

后处理

  1. additionare added in portions
  2. temperaturewith cooling
  3. stirringthe mixture is stirred for 2 hours at room temperature and for a further 5 hours
  4. temperatureat reflux temperature
  5. filtrationThe entire batch is then filtered while hot and
  6. concentrationconcentrated in vacuo