참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Ethane, 1-fluoro-2-iodo- | HCID 69804 | — |
| 반응물 | HCID 178469268 | HCID 178469268 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Ethyl 1-(2-fluoroethyl)-1H-pyrazole-5-carboxylate | HCID 58356443 | 41.1% |
반응 단계
To a solution of ethyl 1H-pyrazole-3-carboxylate (0.77 g) (available from ABCR) in acetonitrile (30 ml) was added cesium carbonate (1.79 g) and the mixture stirred for 5 min when 1-fluoro-2-iodoethane (0.96 g) was added and the mixture stirred at 20° C. for 18 h. The mixture was evaporated and the residue taken up in water (30 ml) and DCM (30 ml) separated by hydrophobic frit and concentrated to ˜5 ml, placed on an SPE cartridge (50 g silica) and eluted with a gradient of ethyl acetate in cyclohexane to give the Ethyl 1-(2-fluoroethyl)-1H-pyrazole-5-carboxylate (0.42 g) as a colourless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08658635B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-a3a04461567e418a95a2dc047cba8e48 |
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| 출처 메모 | uspto-grants-2014_02 |
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