Reacción #1726705

ord-84fa9550a45b4384b436d713367932cc

Ecuación de reacción

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
Rendimiento 80.0%

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ExtracciónThe organics were extracted three times with diethyl ether (total 40 ml)
  2. 2
    Lavadowashed with brine
  3. 3
    Secadodried over magnesium sulfate
  4. 4
    OtroRemoval of solvent

Procedimiento

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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08110568B2uspto-grants-2012_02