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Methylhydrazine → 1-Methyl-3-phenyl-1H-pyrazol-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylhydrazine | HCID 6061 | — |
| 反応物 | Benzoylacetonitrile | HCID 64799 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-Methyl-3-phenyl-1H-pyrazol-5-amine | HCID 517779 | 71.2% |
反応手順
A mixture of benzoyl acetonitrile (2.0 g, 13.778 mmol) and methyl hydrazine (0.698, 15.156 mmol) in methanol (10 mL) was irradiated under microwave conditions at 110° C. for 90 min. The reaction mixture was cooled to rt and poured into rapidly stirred ice cold water. The obtained solid was collected by filtration, dried under vacuum and triturated with a mixture of pentane-hexane (˜10 mL) to yield a white solid (1.7 g, 71%). [1H-NMR (CDCl3, 300 MHz) δ 7.82-7.65 (m, 2H), 7.45-7.20 (m, 3H), 5.90 (s, 1H), 3.75 (s, 3H), 3.55 (s, 2H); LCMS RtA=0.824 min; [M+H]+=174.1]
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08742106B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-13a444bbc6634ce09bcbd8cf08acef13 |
| 出典メモ | uspto-grants-2014_06 |