반응 #1340556

반응 방정식

hydrochloric acid

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

diisopropyl aluminum hydride

ammonium chloride

→

captioned compound

수율 101.5%

3-(3-trifluoromethylphenyl)propanal

수율 101.5%

용매

water

dichloromethane

hexane

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred
2. 2
   기타the resultant was separated into an aqueous layer
3. 3
   추출The aqueous layer was extracted with dichloromethane
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   농축concentrated under reduced pressure

실험 절차

2.40 g of 3-(3-trifluoromethylphenyl)-propionic acid methyl ester synthesized in Step 1 was dissolved in 20 ml of dry dichloromethane. 13 ml of diisopropyl aluminum hydride solution (0.91 M) in hexane was dropped over 5 minutes at −78° C. under an argon atmosphere, and the mixture was stirred at the same temperature for 40 minutes. 50 ml of a saturated ammonium chloride aqueous solution was dropped, and then the mixture was stirred and the temperature was raised to room temperature. 20 ml of water and 5 ml of concentrated hydrochloric acid were added, and the resultant was separated into an aqueous layer and an organic layer. The aqueous layer was extracted with dichloromethane, and the extract was combined with the separated organic layer, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure to afford 2.12 g of the captioned compound as an oil.

출처