Reacción #5334
ord-38557339d9a449aeba84ca978a2ba6b2
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1OtroResulting crystalline precipitates
- 2Filtraciónwere collected by filtration
- 3Lavadowashed with isopropylether
- 4workup.STIRRINGThe suspension was stirred for 30 minutes
- 5Filtracióninsoluble materials were collected by filtration
- 6Otrodried
- 7Otroto give crude crystals
- 8OtroRecrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.)
Procedimiento
A mixture of 4'-methylbiphenyl-2-carboxamide (2.1 g), N-bromo-succinimide (2.5 g) and azobisisobutyronitrate (AIBN; 82 mg) in benzene (20 ml) was stirred for 20 hours at 60° to 70° C. Resulting crystalline precipitates were collected by filtration, washed with isopropylether and suspended in water. The suspension was stirred for 30 minutes, and insoluble materials were collected by filtration and dried to give crude crystals. Recrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.).