Реакция #1563935

ord-56f9c4daa91c44b3b68ba6cd366eaa65

Растворители

Условия реакции

Температура
40°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеreaction mass
  2. 2
    Другоеreaction mass
  3. 3
    Концентрированиеwas concentrated at temperature below 40° C. under reduced pressure
  4. 4
    Другоеto afford Int-11 (50 g) which
  5. 5
    Другоеwas used in the next step without further purification

Методика

A solution of tert-butyl (3-fluoropyridin-4-yl)carbamate (25.0 g, 125 mmol) in MeCN (200 ml), was added O-(2,4-dinitrophenyl)hydroxylamine (26.64 g, 125 mmol) in MeCN (200 ml), drop wise over 30 min at RT, reaction mass was stirred at 40° C. for 12 hrs, reaction mass was concentrated at temperature below 40° C. under reduced pressure to afford Int-11 (50 g) which was used in the next step without further purification.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09402833B2uspto-grants-2016_08