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Hydrochloric Acid → 2-(Piperazin-1-yl)pyridin-3-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-(3-Nitropyridin-2-yl)piperazine | HCID 3778834 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(Piperazin-1-yl)pyridin-3-amine | HCID 10397358 | — |
反応手順
2-(1-piperazinyl)-3-nitropyridine (24.50 g), ethanol (445 ml) and hydrochloric acid (1.2N, 44 ml) are combined and hydrogenated overnight at 40 psi, refilling when necessary. The mixture is filtered through celite, washed with ethanol, chloroform, ethanol and water. The organic solvents are removed with heat and reduced pressure. The remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate. The organic layers are combined, dried over potassium carbonate, filtered and concentrated under reduced pressure to give an oil which slowly solidified upon standing to give 3-amino-2-(1-piperazinyl)pyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05268477 |
| 出典データセット | uspto-grants-1993_12 |
| ORD ID | ord-55e9d79048d24531bc55fa44cf591181 |
| 出典メモ | uspto-grants-1993_12 |