反应 #1973903

反应方程式

compound ( 23 )

8-[4-(4-butoxy-2,3-difluorophenyl)-cyclohexenyl]-1,4-dioxaspiro[4.5]decane

formic acid

water

→

4′-(4-butoxy-2,3-difluorophenyl)-bicyclohexyl-4-one

收率 98.5%

溶剂

toluene

toluene

反应条件

后处理

1. 1
   温度the mixture was heated
2. 2
   温度to reflux for 2 hours
3. 3
   workup.ADDITIONmixed with it
4. 4
   其他had separated into two phases of organic and aqueous phases
5. 5
   萃取the extraction into an organic phase
6. 6
   其他The resulting organic phase was separated
7. 7
   洗涤washed successively with water
8. 8
   干燥a saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over anhydrous magnesium sulfate
9. 9
   workup.DISTILLATIONThen the solvent was distilled off under reduced pressure
10. 10
    其他the residue was purified by recrystallization from heptane solvent
11. 11
    其他dried

实验过程

The compound (23) (7.7 g), formic acid (87%; 8.7 g) and toluene (100 ml) were mixed and the mixture was heated to reflux for 2 hours. After the reaction mixture had been cooled to 30° C., water (200 ml) and toluene (200 ml) were added to the mixture and mixed with it. The mixture was then allowed to stand until it had separated into two phases of organic and aqueous phases, and the extraction into an organic phase was carried out. The resulting organic phase was separated, and washed successively with water, a saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over anhydrous magnesium sulfate. Then the solvent was distilled off under reduced pressure, and the residue was purified by recrystallization from heptane solvent and dried to give 4′-(4-butoxy-2,3-difluorophenyl)-bicyclohexyl-4-one (24) (6.8 g). The yield based on the compound (23) was 99.0%.

来源