反应 #1340556

反应方程式

hydrochloric acid

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

diisopropyl aluminum hydride

ammonium chloride

→

captioned compound

收率 101.5%

3-(3-trifluoromethylphenyl)propanal

收率 101.5%

溶剂

water

dichloromethane

hexane

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred
2. 2
   其他the resultant was separated into an aqueous layer
3. 3
   萃取The aqueous layer was extracted with dichloromethane
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   浓缩concentrated under reduced pressure

实验过程

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.

来源