反应 #2446070

反应方程式

Toluene

p-toluenesulfonic acid monohydrate

1-(4-ethoxy-2,3-difluorophenyl)-4-(3-propylcyclopentyl)cyclohexanol

→

1-ethoxy-2,3-difluoro-4-(4-(3-propylcyclopentyl)cyclohex-1-enyl)benzene

收率 82.0%

溶剂

water

反应条件

后处理

1. 1
   其他obtained in the first step, in a reaction vessel
2. 2
   其他equipped with a Dean-Stark apparatus under an atmosphere of nitrogen
3. 3
   温度The mixture was refluxed for 1.5 hour
4. 4
   其他was removed with a Dean-Stark apparatus
5. 5
   洗涤the reaction solution was washed with water
6. 6
   干燥dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
8. 8
   其他The residue was purified by silica gel chromatography (eluent: ethyl acetate/n-heptane= 1/10 by volume)

实验过程

Toluene (50 ml) and p-toluenesulfonic acid monohydrate (0.15 g) were added to 1-(4-ethoxy-2,3-difluorophenyl)-4-(3-propylcyclopentyl)cyclohexanol (5.0 g) obtained in the first step, in a reaction vessel equipped with a Dean-Stark apparatus under an atmosphere of nitrogen. The mixture was refluxed for 1.5 hour, while forming water was removed with a Dean-Stark apparatus. After the mixture had been cooled to room temperature, the reaction solution was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: ethyl acetate/n-heptane= 1/10 by volume) to give 1-ethoxy-2,3-difluoro-4-(4-(3-propylcyclopentyl)cyclohex-1-enyl)benzene (3.9 g).

来源