関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | N,N-dimethylformamide ethanol | HCID 19794673 | — |
| 反応物 | 1-(5-Fluoro-2-nitrophenyl)piperidine | HCID 53256708 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Dimethyl-(4-nitro-3-piperidin-1-yl-phenyl)-amine | HCID 69312829 | 27% |
反応手順
To a solution of 1-(5-fluoro-2-nitro-phenyl)-piperidine (294 mg, 1.31 mmol, as prepared in the previous step) in 8 mL EtOH-DMF (v/v) was added NaCN (128 mg, 2.6 mmol). The reaction was heated to 130° C. in a sealed tube for 24 h. The reaction was diluted with EtOAc (50 mL) and washed with water (2×50 mL). Chromatography (50% EtOAc-hexane) of the crude product afforded 88 mg (27%) the title compound as well as 78 mg (24%) (1-(5-ethoxy-2-nitro-phenyl)-piperidine as yellow solids. Mass spectrum (ESI, m/z): Calcd. for C13H19N3O2, 250.1 (M+H), found 250.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07427683B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-86b810c8a16945c2aa27b3ff2b97ca07 |
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| 出典メモ | uspto-grants-2008_09 |
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