تفاعل #1726705

ord-84fa9550a45b4384b436d713367932cc

معادلة التفاعل

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
المردود 80.0%

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe organics were extracted three times with diethyl ether (total 40 ml)
  2. 2
    غسيلwashed with brine
  3. 3
    تجفيفdried over magnesium sulfate
  4. 4
    أخرىRemoval of solvent

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08110568B2uspto-grants-2012_02