反応 #1885021

反応方程式

2-chloro-5-chloromethylpyridine

2,2-difluoroethan-1-amine

triethylamine

→

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

収率 53.9%

溶媒

acetonitrile

反応条件

後処理

1. 1
   濃縮After concentrating the reaction mixture under reduced pressure, it
2. 2
   洗浄washed with ethyl acetate
3. 3
   抽出extracted repeatedly with ethyl acetate
4. 4
   濃縮Concentrating the organic phase under reduced pressure

実験手順

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.

出典