反应 #1726705

ord-84fa9550a45b4384b436d713367932cc

反应方程式

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
收率 80.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取The organics were extracted three times with diethyl ether (total 40 ml)
  2. 2
    洗涤washed with brine
  3. 3
    干燥dried over magnesium sulfate
  4. 4
    其他Removal of solvent

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08110568B2uspto-grants-2012_02