참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 2-Hydrazinopyridine | HCID 78645 | — |
| 반응물 | Aminocrotononitrile | HCID 86589747 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-5-amine | HCID 735132 | 90% |
반응 단계
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 mixture was heated under reflux for 3.5 hours. After the mixture was allowed to cool to room temperature, the reaction solvent was evaporated under reduced pressure and water was added to the residue. After the solution was made basic by the addition of an aqueous sodium hydroxide solution, 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. Purification of the residue by silica gel column chromatography (ethyl acetate) gave the title compound (156.3 g, 90% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06949648B2 |
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| 출처 데이터셋 | uspto-grants-2005_09 |
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| ORD ID | ord-608a2beee47140a2a93a373efc43f977 |
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| 출처 메모 | uspto-grants-2005_09 |
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