Реакция #1726705

ord-84fa9550a45b4384b436d713367932cc

Уравнение реакции

N#Cc1cnn(-c2cccc([N+](=O)[O-])c2)c1N
5-amino-1-(3′-nitrophenyl)-4-cyanopyrazole
O=P(O)(O)O
phosphoric acid
[NH4+].[OH-]
ammonium hydroxide
Nc1ccnn1-c1cccc([N+](=O)[O-])c1
5-amino-1-(3′-nitrophenyl)-pyrazole
Выход 80.0%

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ЭкстракцияThe organics were extracted three times with diethyl ether (total 40 ml)
  2. 2
    Промывкаwashed with brine
  3. 3
    Сушкаdried over magnesium sulfate
  4. 4
    ДругоеRemoval of solvent

Методика

5-amino-1-(3′-nitrophenyl)-4-cyanopyrazole (559 mg, 2.44 mmol) and phosphoric acid (86%, 6 ml) were refluxed at 170° C. for 15 h. The reaction was cooled to room temperature and neutralized with ammonium hydroxide. The organics were extracted three times with diethyl ether (total 40 ml), washed with brine, and dried over magnesium sulfate. Removal of solvent gave 5-amino-1-(3′-nitrophenyl)-pyrazole as a yellow powder (398 mg, 80% yield).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08110568B2uspto-grants-2012_02