反応 #712923

反応方程式

ammonia

5-nitro-3-pyrazolecarboxylic acid

carbonyldiimidazole

→

3-nitro-1H-pyrazole-5-carboxamide

収率 48.0%

溶媒

MeOH

DMF

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction mixture was stirred at rt overnight
2. 2
   濃縮The mixture was concentrated under reduced pressure
3. 3
   その他to afford the crude product which
4. 4
   洗浄was then washed with ether

実験手順

To a solution of 5-nitro-3-pyrazolecarboxylic acid (6.28 mg, 40 mmol) in DMF (30 mL) was added carbonyldiimidazole (12.96 mg, 80 mmol) The mixture was allowed to stir for 30 min, and ammonia in MeOH (2M, 60 mL) was added. The reaction mixture was stirred at rt overnight. The mixture was concentrated under reduced pressure to afford the crude product which was then washed with ether to afford 3-nitro-1H-pyrazole-5-carboxamide (3.0 g, 48%), which was used directly in the next step without further purification. LC-MS (ESI) m/z 155 (M−H)−.

出典