Reacción #5334

ord-38557339d9a449aeba84ca978a2ba6b2

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroResulting crystalline precipitates
  2. 2
    Filtraciónwere collected by filtration
  3. 3
    Lavadowashed with isopropylether
  4. 4
    workup.STIRRINGThe suspension was stirred for 30 minutes
  5. 5
    Filtracióninsoluble materials were collected by filtration
  6. 6
    Otrodried
  7. 7
    Otroto give crude crystals
  8. 8
    OtroRecrystallization 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.).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05243054uspto-grants-1993_09