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 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Methyl N-cyano-3-furancarboximidate | HCID 19734520 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-cyano-N'-(2-nitroxyethyl)-3-furancarboximidamide | HCID 19754250 | 8.2% |
反応手順
Methyl N-cyano-3-furancarboximidate (0.5 g, 3.3 mmol) was dissolved in methanol (10 ml), and 2 nitroxyethylamine nitrate (0.84 g, 5.0 mmol) and sodium methoxide (0.27 g, 5.0 mmol) were added. The mixture was stirred at room temperature for 26 hours. After the reaction was completed, the reaction solution was concentrated under reduced pressure, and the residue thus obtained was extracted with chloroform (60 ml×3). The chloroform layer was washed with water (100 ml), dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residual concentrate was subjected to chromatography on a silica gel column (WAKO GEL C 200, 20 g) eluting with chloroform-methanol (100:1). The eluted fractions were concentrated under reduced pressure and crystallized from methanol-diethyl ether to give the title compound (0.06 g, 0.27 mmol, yield: 8%) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05166347 |
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| 出典データセット | uspto-grants-1992_11 |
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| ORD ID | ord-72ee8c912729413a94d38a7e76dc96e3 |
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| 出典メモ | uspto-grants-1992_11 |
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