関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Benzyl-4-(4-nitrophenyl)piperazine | HCID 2747427 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-(4-Benzylpiperazin-1-yl)aniline | HCID 737259 | — |
反応手順
Iron powder (5.4 g, 97 mmol, 4 equiv) is added portionwise to an 80° C. mixture of 1-benzyl-4-(4-nitro-phenyl)-piperazine (7.2 g, 24.2 mmol), EtOH (150 mL), H2O (40 mL), and AcOH (20 mL). The reaction mixture is stirred for 1.75 h at 80° C., allowed to cool to RT, and concentrated. The residue is diluted with EtOAc and an aqueous saturated solution of Na2CO3. The layers are separated and the aqueous phase is extracted with EtOAc. The combined organic phase is washed with brine, dried (Na2SO4), filtered and concentrated to afford the title compound: ES-MS: 268.3 [MH]+; single peak at tR=1.30 min (system 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08759517B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-9ac1155e7ef04fc7ab35e1595741496c |
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| 出典メモ | uspto-grants-2014_06 |
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