反应 #1929012

反应方程式

water

thionyl chloride

4-propylcyclohexanol

DMF

→

1-chloro-4-propylcyclohexane

溶剂

toluene

反应条件

后处理

1. 1
   温度the mixture is heated to reflux
2. 2
   温度is heated for a further 4 h
3. 3
   温度After cooling
4. 4
   其他the organic phase is separated off
5. 5
   萃取The aqueous phase is extracted with toluene
6. 6
   洗涤the combined organic phases are washed with water and saturated sodium chloride solution
7. 7
   其他The solution is dried
8. 8
   浓缩concentrated to dryness
9. 9
   其他The crude product is purified by column chromatography (SiO2, n-heptane)

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.

来源