반응 #1885021

반응 방정식

2-chloro-5-chloromethylpyridine

2,2-difluoroethan-1-amine

triethylamine

→

N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethan-1-amine

수율 53.9%

용매

acetonitrile

반응 조건

후처리

1. 1
   농축After concentrating the reaction mixture under reduced pressure, it
2. 2
   세척washed with ethyl acetate
3. 3
   추출extracted repeatedly with ethyl acetate
4. 4
   농축Concentrating the organic phase under reduced pressure

실험 절차

At 45° C., 41.57 g (256.6 mmol) of 2-chloro-5-chloromethylpyridine, 20.80 g (256.6 mmol) of 2,2-difluoroethan-1-amine and 35.8 ml (256.6 mmol) of triethylamine are stirred in 500 ml of acetonitrile for 21 hours. After concentrating the reaction mixture under reduced pressure, it is taken up with 1 N aqueous hydrochloric acid and washed with ethyl acetate. The aqueous phase is alkalized with 2.5 N aqueous sodium hydroxide solution and extracted repeatedly with ethyl acetate. Concentrating the organic phase under reduced pressure affords 28.6 g (53% of theory) of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethan-1-amine.

출처