関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Diphenylethylamine | HCID 26482 | — |
| 反応物 | 3-Pyridinecarboximidic acid, N-cyano-, 1-methylethyl ester | HCID 10081201 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-cyano-N'-(1,2-diphenylethyl)-3-pyridinecarboximidamide | HCID 19734548 | 58% |
反応手順
Isopropyl N-cyano-3-pyridinecarboximidate (0.60 g, 3.2 mmol) was dissolved in methanol (10 ml), and 1,2-diphenylethylamine (0.69 g, 3.5 mmol) was added. The mixture was stirred at room temperature for 45 minutes. After the reaction was completed, the reaction solution was concentrated under reduced pressure. The residual concentrate thus obtained was subjected to chromatography on a silica gel column (WAKO GEL C-200, 50 g) eluting with chloroform-methanol (100:1). The eluted fractions were concentrated under reduced pressure to give N-cyano-N'-(1,2-diphenylethyl)-3-pyridinecarboximidamide (0.60 g, 1.8 mmol, yield: 58%) as colorless syrup. Next, to this syrup was added a 5% hydrogen chloride solution in methanol (2.5 ml). The solution was crystallized from a methanol-diethyl ether to give N-cyano-N'-(1,2-diphenylethyl)-3-pyridinecarboximidamide hydrochloride as colorless powder.
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-81818e51cbb5444d837f384c188e7761 |
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| 出典メモ | uspto-grants-1992_11 |
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