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Ethanol, 2-amino-, 1-nitrate, nitrate (1:1) → N-cyano-N'-(2-nitroxyethyl)-4-pyridinecarboximidamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol, 2-amino-, 1-nitrate, nitrate (1:1) | HCID 78397 | — |
| 反応物 | Isopropyl N-cyano-4-pyridinecarboximidate | HCID 10012715 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-cyano-N'-(2-nitroxyethyl)-4-pyridinecarboximidamide | HCID 10059957 | 61.5% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05166347 |
| 出典データセット | uspto-grants-1992_11 |
| ORD ID | ord-d01f77a329184a65851e0541cd12a4d8 |
| 出典メモ | uspto-grants-1992_11 |