반응 #1340555

반응 방정식

3-(trifluoromethyl) cinnamic acid

ethanol

→

captioned compound

3-(3-trifluoromethylphenyl)-propionic acid methyl ester

반응 조건

후처리

1. 1
   기타Palladium/carbon was separated by filtration
2. 2
   농축the filtrate was concentrated under reduced pressure
3. 3
   workup.ADDITION20 ml of methanol and 4 drops of concentrated sulfuric acid were added
4. 4
   workup.STIRRINGthe mixture was stirred at 60° C. for 2 hours
5. 5
   workup.WAITleft
6. 6
   온도to cool down
7. 7
   농축After concentration under reduced pressure, 20 ml of a saturated sodium bicarbonate aqueous solution
8. 8
   workup.ADDITIONwas added
9. 9
   추출the resultant was extracted with 20 ml of dichloromethane
10. 10
    건조The extract was dried with anhydrous sodium sulfate
11. 11
    농축concentrated under reduced pressure

실험 절차

A mixture of 2.20 g of 3-(trifluoromethyl) cinnamic acid, 166 mg of palladium/carbon (10%, wet), and 40 ml of ethanol was stirred overnight under a hydrogen atmosphere at 1 atm. Palladium/carbon was separated by filtration, and the filtrate was concentrated under reduced pressure. 20 ml of methanol and 4 drops of concentrated sulfuric acid were added and the mixture was stirred at 60° C. for 2 hours, and then left to cool down. After concentration under reduced pressure, 20 ml of a saturated sodium bicarbonate aqueous solution was added, and the resultant was extracted with 20 ml of dichloromethane. The extract was dried with anhydrous sodium sulfate and then concentrated under reduced pressure to afford 2.40 g of the captioned compound as an oil.

출처