反応 #712924

反応方程式

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

phosphorus oxychloride

→

3-nitro-1H-pyrazole-5-carbonitrile

溶媒

pyridine

反応条件

後処理

1. 1
   workup.ADDITIONThe reaction mixture was diluted with ice
2. 2
   抽出extracted with DCM (100 mL)
3. 3
   乾燥dried over sodium sulfate
4. 4
   ろ過filtered
5. 5
   濃縮concentrated under reduced pressure

実験手順

3-nitro-1H-pyrazole-5-carboxamide (3.0 g, 19.2 mmol) in pyridine (30 mL) was treated with phosphorus oxychloride (5.9 g) and the resultant solution was stirred for 3 h at rt. The reaction mixture was diluted with ice, then extracted with DCM (100 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure to afford the crude 3-nitro-1H-pyrazole-5-carbonitrile, which was used directly in the next step without further purification. LC-MS (ESI) m/z 137 (M−H)−.

出典