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Dimethyl Sulfoxide → 1-[5-(4-Methyl-pyrazol-1-yl)-2-nitro-phenyl]-piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(5-Fluoro-2-nitrophenyl)piperidine | HCID 53256708 | — |
| 反応物 | HCID 178428694 | HCID 178428694 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-[5-(4-Methyl-pyrazol-1-yl)-2-nitro-phenyl]-piperidine | HCID 68684342 | 95% |
反応手順
A solution of 1-(5-fluoro-2-nitro-phenyl)-piperidine (98 mg, 0.43 mmol, as prepared in Example 22, step (a), 3-methylpyrazole (49.2 mg, 0.6 mmol), and NaOH (22.4 mg, 0.56 mmol) were heated in 3 mL of DMSO at 90° C. overnight. The reaction was diluted with EtOAc (50 mL), washed with water (2×50 mL), dried (Na2SO4) and concentrated in vacuo to afford 117 mg (95%) the title compound as a yellow solid. Mass spectrum (ESI, m/z): Calcd. for C15H18N4O2 287.1 (M+H), found 287.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07705042B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-e73a654692564a71ae05df4223126f37 |
| 出典メモ | uspto-grants-2010_04 |