반응 #1973903

반응 방정식

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

수율 98.5%

용매

toluene

toluene

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도to reflux for 2 hours
3. 3
   workup.ADDITIONmixed with it
4. 4
   기타had separated into two phases of organic and aqueous phases
5. 5
   추출the extraction into an organic phase
6. 6
   기타The resulting organic phase was separated
7. 7
   세척washed successively with water
8. 8
   건조a 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
    기타the residue was purified by recrystallization from heptane solvent
11. 11
    기타dried

실험 절차

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%.

출처