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Triethylamine → N-cyano-N'-(2-nitroxyethyl)-2-thiophenecarboximidamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethanol, 2-amino-, 1-nitrate, nitrate (1:1) | HCID 78397 | — |
| 反応物 | 2-Thiophenecarboximidic acid, N-cyano-, methyl ester | HCID 10241147 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-cyano-N'-(2-nitroxyethyl)-2-thiophenecarboximidamide | HCID 10082992 | 40.5% |
反応手順
Methyl N-cyano-2-thiophenecarboximidate (0.32 g, 1.9 mmol) was dissolved in methanol (3 ml), and 2-nitroxyethylamine nitrate (0.34 g, 2.0 mmol) and triethylamine (0.20 g, 2.0 mmol) were added. The mixture was stirred at room temperature for 17 hours. After the reaction was completed, the reaction solution was concentrated under reduced pressure, and the residue thus obtained was subjected to chromatography on a silica gel column (WAKO GEL C-200, 25 g) eluting with ethyl acetate. The eluted fractions were concentrated under reduced pressure and crystallized from ethyl acetate-hexane to give the title compound (0.18 g, 0.77 mmol, yield: 40%) as colorless crystals.
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-7af2253643b74fdb9bbd371bbe2c6e39 |
| 出典メモ | uspto-grants-1992_11 |