反応 #1726705

ord-84fa9550a45b4384b436d713367932cc

反応方程式

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
収率 80.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出The organics were extracted three times with diethyl ether (total 40 ml)
  2. 2
    洗浄washed with brine
  3. 3
    乾燥dried over magnesium sulfate
  4. 4
    その他Removal of solvent

実験手順

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).

出典

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