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Hexahydro-1H-azepine-1-acetonitrile → Hexahydro-1H-azepine-1-ethanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexahydro-1H-azepine-1-acetonitrile | HCID 41164 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Hexahydro-1H-azepine-1-ethanamine | HCID 40002 | 35.3% |
反応手順
A mixture of nitrile 290 (5.58 g, 40.4 mmol) and Raney Nickel (50% w/w in water, ca. 5 mL) in EtOH (50 mL) and cNH3 (4 mL) was stirred under H2 (60 psi) for 16 h. The mixture was filtered through Celite, washed with EtOH (3×10 mL) and the solvent evaporated to give crude diamine 291 as an oil (2.03 g, 35%) which was used without further purification: 1H NMR δ 2.72 (t, J=6.1 Hz, 2H, CH2N), 2.60-2.68 (m, 4H, 2×CH2N), 2.53 (t, J=6.1 Hz, 2H, CH2N), 1.55-1.66 (m, 10H, 4×CH2, NH2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07989451B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-ff3b8ebcc95e4f218406e6e70ae91b26 |
| 出典メモ | uspto-grants-2011_08 |