Reacción #2006433
ord-15e8da58edcf48d08504425a6efc6c91
Ecuación de reacción
4-bromo-2,2′-bipyridyl-N-oxide
PCl3
→
4-bromo-2,2′-bipyridyl
Rendimiento 85.0%
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Otroat room temperature
- 2TemperaturaThe mixture was refluxed for 2 h under N2
- 3OtroThe aqueous layer was separated
- 4ExtracciónThe CHCl3, layer was extracted three times with H2O (3×60 mL)
- 5FiltraciónThe resulting white precipitate was collected by suction filtration
- 6Lavadowashed with H2O (30 mL)
- 7Otrodried 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%.