反应 #1109822

反应方程式

(2RS)-(3,4-dichlorophenyl)[(4RS)-2,2-dimethyl-1,3-dioxolan-4-yl]ethanenitrile

diisobutylaluminum hydride toluene

→

title compound

收率 100.6%

(2RS)-2-(3,4-dichlorophenyl)-2-[(4RS)-2,2-dimethyl-1,3-dioxolan-4-yl]ethanamine

收率 100.6%

溶剂

toluene

反应条件

后处理

1. 1
   其他The reaction was quenched with water at −78° C.
2. 2
   workup.ADDITIONaqueous potassium carbonate solution was added
3. 3
   萃取the mixture was extracted with ethyl acetate
4. 4
   洗涤The organic layer was washed with brine
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   其他the solvent was evaporated

实验过程

To a solution of (2RS)-(3,4-dichlorophenyl)[(4RS)-2,2-dimethyl-1,3-dioxolan-4-yl]ethanenitrile (10.0 g) in toluene (100 ml) was added dropwise 1.5 M diisobutylaluminum hydride/toluene solution (51.3 under nitrogen purging at −78° C., and the mixture was stirred for 3 hr. The reaction was quenched with water at −78° C., aqueous potassium carbonate solution was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated to give the title compound (10.2 g) as a colorless oil. This was used for the next step without purification.

来源