Реакция #5334

ord-38557339d9a449aeba84ca978a2ba6b2

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеResulting crystalline precipitates
  2. 2
    Фильтрацияwere collected by filtration
  3. 3
    Промывкаwashed with isopropylether
  4. 4
    workup.STIRRINGThe suspension was stirred for 30 minutes
  5. 5
    Фильтрацияinsoluble materials were collected by filtration
  6. 6
    Другоеdried
  7. 7
    Другоеto give crude crystals
  8. 8
    ДругоеRecrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.)

Методика

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.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05243054uspto-grants-1993_09