関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | N-[3-(4-methylpiperazin-1-yl)propyl]-4-nitro-1-aminobenzene | HCID 21975010 | — |
| 触媒 | Nickel | HCID 935 | — |
| 生成物 | 1-(4-Aminophenyl)piperidin-4-ol | HCID 16792107 | 51% |
反応手順
A 50 mL round bottom flask was charged with [3-(4-Methyl-piperazin-1-yl)-propyl]-(4-nitro-phenyl)-amine (0.742 g, 3.34 mmol) and dissolved into EtOH (20 mL). Hydrazine Hydrate (0.642 mL, 20.04 mmol) was then added. Excess RaNi was then added in dropwise until the solution stopped bubbling. The suspension was then allowed to stir for an additional 15 minutes at 65° C. The suspension was cooled to rt and then filtered over celite. The celite was washed with MeOH (˜20 mL) and the combined organic solutions were then concentrated in vacuo. The crude oil was then purified over silica (3% Chloroform/Hexanes to 10% Chloroform/Hexanes) affording pure 1-(4-amino-phenyl)-piperidin-4-ol as a light brown oil in 51% yield (0.327 g, 1.71 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07692005B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-07b8551954aa446ba8517d6fd8f02df7 |
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| 出典メモ | uspto-grants-2010_04 |
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