Реакция #4331

ord-6690a163904649839ee51f83c59f74e3

Растворители

Условия реакции

Температура
96°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONare added
  2. 2
    ТемператураAfter cooling it
  3. 3
    ДругоеThe expected product precipitates
  4. 4
    ФильтрацияAfter being filtered off
  5. 5
    Промывкаwashed
  6. 6
    Другоеis recrystallized from 250 ml of acetic acid

Методика

To 310 ml of acetic acid diluted with 160 ml of water are added: 1.5 g of sodium nitrite, 0.16 mole (42 g) of 2,5-difluoro-N-benzenesulphonylaniline prepared in the previous stage and 0.94 mole (39 ml) of nitric acid (d=1.52). The reaction mixture is heated to 96° C. for 1 hour. After cooling it is poured onto 1 kg of ice and water. The expected product precipitates. After being filtered off and washed to neutrality it is recrystallized from 250 ml of acetic acid; it melts at 176° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04725283uspto-grants-1988_02