참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | Ethyl 3-acetyl-4-oxopentanoate | HCID 87820 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | ethyl 2-(3,5-dimethyl-1H-pyrazol-4-yl)acetate | HCID 16394806 | 72% |
반응 단계
To a solution of ethyl 3-acetyl-4-oxopentanoate (synthesized as described D. P. Shrout and D. A. Lightner, Synth. Commun. 20 (1990), 2075) (9.676 g, 51.96 mmol) in ethanol, at 0° C., was added slowly a solution of hydrazine hydrate (2.990 g, 59.75 g) in absolute ethanol. The reaction mixture was warmed to room temperature and stirred for 2 hours. After removing ethanol under vacuum, dichloromethane and water were added to the crude product and the organic layer was separated. The aqueous layer was extracted further with dichloromethane and the combined organic extracts were washed with water. After drying over MgSO4 and evaporation of the solvent under reduced pressure, the pyrazole was isolated as a yellow oil. Yield: 72% (6.777 g, 37.2 mmol).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08372379B2 |
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| 출처 데이터셋 | uspto-grants-2013_02 |
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| ORD ID | ord-9c886412d52e4145be71feddcd8fb175 |
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| 출처 메모 | uspto-grants-2013_02 |
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