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Putrescine → 4,5,6,7-tetrahydro-2[2-(4-pyridyl)ethyl]-1H-1,3-diazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Putrescine | HCID 1045 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | 4-Pyridinepropanenitrile | HCID 7330461 | — |
| 反応物 | 1,4-Diaminobutane di-p-toluenesulfonate | HCID 20239771 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4,5,6,7-tetrahydro-2[2-(4-pyridyl)ethyl]-1H-1,3-diazepine | HCID 13281194 | 93.6% |
反応手順
The mixture of 4-[2-cyanoethyl]pyridine (1.32 g, 0.01M), 1,4-diaminobutane (0.88 g, 0.01M) and 1,4-diaminobutane di-p-toluenesulfonate (4.32 g, 0.01M) was heated at about 190° to about 200° C. for 4 hrs. The residue was stirred with ethanol (20 ml) which contained EtONa (0.02M) and filtered. The filtrate was concentrated and distilled at 0.07 mmHg and a temperature of about 180° to about 200° C. to give 4,5,6,7-tetrahydro-2[2-(4-pyridyl)ethyl]-1H-1,3-diazepine (1.9 g, 93% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04605744 |
| 出典データセット | uspto-grants-1986_08 |
| ORD ID | ord-b0e070306c3c4a50b63785f89189f544 |
| 出典メモ | uspto-grants-1986_08 |