Reaktion #1885021

Reaktionsgleichung

2-chloro-5-chloromethylpyridine

2,2-difluoroethan-1-amine

triethylamine

→

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

Ausbeute 53.9%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenAfter concentrating the reaction mixture under reduced pressure, it
2. 2
   Waschenwashed with ethyl acetate
3. 3
   Extraktionextracted repeatedly with ethyl acetate
4. 4
   EinengenConcentrating the organic phase under reduced pressure

Vorschrift

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.

Quelle