HRID46485

反应详情

EQUATION

反应方程式

HRID 46485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(5-Methyl-4-imidazolylmethylthio)ethanol (0.34 g, 2 mmol) and thionyl chloride (0.238 g, 2 mmol) were heated together, with stirring, at reflux temperature in chloroform (10 ml) for one hour, giving a grey solution and a green oil. A second equivalent of thionyl chloride (0.238 g) was added at reflux temperature and immediately the oil went into solution and a solid started to crystallise. After a further 15 minutes at reflux temperature the mixture was cooled and the solid collected (0.395 g). Recrystallisation from acetonitrile gave 1-chloro-2-(5-methyl-4-imidazolylmethylthio)ethane hydrochloride, m.p. 163°-165°, (0.29 g).

WORKUP

后处理

  1. customgiving a grey solution
  2. temperatureat reflux temperature
  3. customto crystallise
  4. temperatureAfter a further 15 minutes at reflux temperature the mixture
  5. temperaturewas cooled
  6. customthe solid collected (0.395 g)
  7. customRecrystallisation from acetonitrile