Réaction #5334

ord-38557339d9a449aeba84ca978a2ba6b2

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreResulting crystalline precipitates
  2. 2
    Filtrationwere collected by filtration
  3. 3
    Lavagewashed with isopropylether
  4. 4
    workup.STIRRINGThe suspension was stirred for 30 minutes
  5. 5
    Filtrationinsoluble materials were collected by filtration
  6. 6
    Autredried
  7. 7
    Autreto give crude crystals
  8. 8
    AutreRecrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.)

Mode opératoire

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.).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05243054uspto-grants-1993_09