Reaktion #1340555
ord-632fe13c58be4ec886ff11dd65f31167
Reaktionsgleichung
Reagenzien
Reaktionsbedingungen
Aufarbeitung
- 1SonstigePalladium/carbon was separated by filtration
- 2Einengenthe filtrate was concentrated under reduced pressure
- 3workup.ADDITION20 ml of methanol and 4 drops of concentrated sulfuric acid were added
- 4workup.STIRRINGthe mixture was stirred at 60° C. for 2 hours
- 5workup.WAITleft
- 6Temperaturto cool down
- 7EinengenAfter concentration under reduced pressure, 20 ml of a saturated sodium bicarbonate aqueous solution
- 8workup.ADDITIONwas added
- 9Extraktionthe resultant was extracted with 20 ml of dichloromethane
- 10TrocknenThe extract was dried with anhydrous sodium sulfate
- 11Einengenconcentrated under reduced pressure
Vorschrift
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.