تفاعل #1973903

معادلة التفاعل

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

المردود 98.5%

المذيبات

toluene

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةto reflux for 2 hours
3. 3
   workup.ADDITIONmixed with it
4. 4
   أخرىhad separated into two phases of organic and aqueous phases
5. 5
   استخلاصthe extraction into an organic phase
6. 6
   أخرىThe resulting organic phase was separated
7. 7
   غسيلwashed successively with water
8. 8
   تجفيفa 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
    أخرىthe residue was purified by recrystallization from heptane solvent
11. 11
    أخرىdried

الإجراء التجريبي

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%.

المصدر