Reacción #1563935

ord-56f9c4daa91c44b3b68ba6cd366eaa65

Ecuación de reacción

CC(C)(C)OC(=O)Nc1ccncc1F
tert-butyl (3-fluoropyridin-4-yl)carbamate
NOc1ccc([N+](=O)[O-])cc1[N+](=O)[O-]
O-(2,4-dinitrophenyl)hydroxylamine
CC(C)(C)OC(=O)Nc1cc[n+](N)cc1F.O=[N+]([O-])c1ccc([O-])c([N+](=O)[O-])c1
1-amino-4-((tert-butoxycarbonyl)amino)-3-fluoropyridin-1-ium 2,4-dinitrophenolate

Disolventes

Condiciones de reacción

Temperatura
40°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09402833B2uspto-grants-2016_08