反応 #1340555

反応方程式

3-(trifluoromethyl) cinnamic acid

ethanol

→

captioned compound

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

反応条件

後処理

1. 1
   その他Palladium/carbon was separated by filtration
2. 2
   濃縮the 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
   温度to cool down
7. 7
   濃縮After concentration under reduced pressure, 20 ml of a saturated sodium bicarbonate aqueous solution
8. 8
   workup.ADDITIONwas added
9. 9
   抽出the resultant was extracted with 20 ml of dichloromethane
10. 10
    乾燥The extract was dried with anhydrous sodium sulfate
11. 11
    濃縮concentrated under reduced pressure

実験手順

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.

出典