反应详情

Isopropyl N-cyano-3-pyridinecarboximidate (0.50 g, 2.6 mmol) was dissolved in methanol (10 ml), and 2-nitroxyethylamine nitrate (0.49 g, 2.9 mmol) and sodium methoxide (0.16 g, 2.9 mmol) were added. The mixture was stirred at room temperature for 10 minutes. After the reaction was completed, the reaction solution was concentrated under reduced pressure, and the residue was extracted with dichloromethane (50 ml×3). The dichloromethane layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The concentrated residue was crystallized from dichloromethane-diethyl ether to give the title compound (0.48 g, 2.1 mmol, yield: 79%) as colorless needles.

1. concentrationthe reaction solution was concentrated under reduced pressure
2. extractionthe residue was extracted with dichloromethane (50 ml×3)
3. dry with materialThe dichloromethane layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe concentrated residue was crystallized from dichloromethane-diethyl ether