HRID1841830

反应详情

EQUATION

反应方程式

HRID 1841830 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100.0 g (0.70 mol) of 4-propylcyclohexanol are initially introduced in 1200 ml of toluene together with 2.7 ml of DMF, and the mixture is heated to reflux. 255 ml (3.52 mol) of thionyl chloride are carefully metered in, and the batch is heated for a further 4 h. After cooling, the mixture is added to water, and the organic phase is separated off. The aqueous phase is extracted with toluene, and the combined organic phases are washed with water and saturated sodium chloride solution. The solution is dried using sodium sulfate and concentrated to dryness. The crude product is purified by column chromatography (SiO2, n-heptane), giving 1-chloro-4-propylcyclohexane as a colourless liquid.

WORKUP

后处理

  1. temperaturethe mixture is heated to reflux
  2. temperatureis heated for a further 4 h
  3. temperatureAfter cooling
  4. customthe organic phase is separated off
  5. extractionThe aqueous phase is extracted with toluene
  6. washthe combined organic phases are washed with water and saturated sodium chloride solution
  7. customThe solution is dried
  8. concentrationconcentrated to dryness
  9. customThe crude product is purified by column chromatography (SiO2, n-heptane)