関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Hydrazinopyridine | HCID 78645 | — |
| 反応物 | Aminocrotononitrile | HCID 86589747 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine | HCID 735132 | 90% |
反応手順
To an ice-cold solution of aminocrotononitrile (82 g, 1.0 mol) and 2-hydrazinopyridine (120 g, 1.1 mol) in ethanol (300 mL) was added acetic acid (132 g, 2.2 mol), and the solution was heated under reflux for 3.5 hours. The solution was cooled to room temperature, and the solution was concentrated under reduced pressure, and water was added to the residue. The solution was made basic by the addition of an aqueous sodium hydroxide solution, and organic matter was extracted with ethyl acetate. The extract was washed with saturated brine and water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to give the title compound (156.3 g, 90% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06949648B2 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-11a61191044d4726b27d7684b8576fea |
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| 出典メモ | uspto-grants-2005_09 |
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