Reacción #2487392

ord-df8e613e5a0e4961a1f33ca455f88d54

Ecuación de reacción

[O-][n+]1ccc(Br)cc1-c1ccccn1
4-bromo-2,2′-bipyridyl-N-oxide
ClP(Cl)Cl
PCl3
Brc1ccnc(-c2ccccn2)c1
4-bromo-2,2′-bipyridyl
Rendimiento 85.0%

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroat room temperature
  2. 2
    TemperaturaThe mixture was refluxed for 2 h under N2
  3. 3
    OtroThe aqueous layer was separated
  4. 4
    ExtracciónThe CHCl3, layer was extracted three times with H2O (3×60 mL)
  5. 5
    FiltraciónThe resulting white precipitate was collected by suction filtration
  6. 6
    Lavadowashed with H2O (30 mL)
  7. 7
    Otrodried under vacuum at 50° C. for 24 h

Procedimiento

To a stirred suspension of 4-bromo-2,2′-bipyridyl-N-oxide in 60 mL CHCl3, was added 12 mL PCl3, at room temperature. The mixture was refluxed for 2 h under N2 and then cooled to room temperature. The reaction mixture was poured into 100 mL ice/water. The aqueous layer was separated and saved. The CHCl3, layer was extracted three times with H2O (3×60 mL) and then discarded. The combined aqueous solution was neutralized with NaHCO3 powder to about pH 7-8. The resulting white precipitate was collected by suction filtration, washed with H2O (30 mL) and then dried under vacuum at 50° C. for 24 h. Yield: 85%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08795490B2uspto-grants-2014_08