Ethanol, 2-amino-, 1-nitrate, nitrate (1:1) → N-cyano-N'-(2-nitroxyethyl)-4-pyridinecarboximidamide

Isopropyl N-cyano-4-pyridinecarboximidate (0.50 g, 2.6 mmol) was dissolved in methanol (10 ml), and 2-nitroxyethylamine nitrate (0.57 g, 2.9 mmol) and sodium methoxide (0.18 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. The residue thus obtained was extracted with dichloromethane (50 ml×3). The dichloromethane layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residual concentrate was crystallized from dichloromethane-diethyl ether to give the title compound (0.37 g, 1.6 mmol, yield: 61%) as colorless needles.

1. concentrationthe reaction solution was concentrated under reduced pressure
2. customThe residue thus obtained
3. extractionwas extracted with dichloromethane (50 ml×3)
4. dry with materialThe dichloromethane layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. concentrationThe residual concentrate
7. customwas crystallized from dichloromethane-diethyl ether

ORD-Eintrag

ord-d01f77a329184a65851e0541cd12a4d8

Quelldatensatz

uspto-grants-1992_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05166347