Реакция #1885021

ord-ea1ab50375b34e25b281175bbcaebf43

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    КонцентрированиеAfter concentrating the reaction mixture under reduced pressure, it
  2. 2
    Промывкаwashed with ethyl acetate
  3. 3
    Экстракцияextracted repeatedly with ethyl acetate
  4. 4
    КонцентрированиеConcentrating the organic phase under reduced pressure

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08343893B2uspto-grants-2013_01