反应 #2348092

反应方程式

water

p-toluenesulfonic acid monohydrate

compound ( 7 )

1-(2,3-difluoro-4-ethoxy-6-methylphenyl)-2-(4-pentylcyclohexyl)ethanol

water

→

1-(2,3-difluoro-4-ethoxy-6-methylphenyl)-2-(4-pentylcyclohexyl)ethene

溶剂

toluene

反应条件

后处理

1. 1
   温度the mixture was heated
2. 2
   其他After terminating
3. 3
   其他the reaction
4. 4
   萃取the aqueous layer was extracted with toluene
5. 5
   洗涤washed with saturated saline
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 resulting residue was purified by silica gel column chromatography
9. 9
   其他subjected to recrystallization

实验过程

0.55 g of p-toluenesulfonic acid monohydrate was added to the compound (7) having been dissolved in 120 mL of toluene, and the mixture was heated under stirring by using a Dean-Stork trap until completion of azeotrope of water. After terminating the reaction by adding water, the aqueous layer was extracted with toluene, washed with saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified by silica gel column chromatography and then subjected to recrystallization to obtain 6.53 g of 1-(2,3-difluoro-4-ethoxy-6-methylphenyl)-2-(4-pentylcyclohexyl)ethene (Compound 1-1-3-18) as colorless crystals.

来源