참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Selectfluor | HCID 2724933 | — |
| 반응물 | ethyl 3-(tert-butyl)-1-methyl-1H-pyrazole-5-carboxylate | HCID 2799344 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester | HCID 67413334 | — |
반응 단계
5-tert-Butyl-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester (210 mg, 1.00 mmol) was added dropwise to a stirred solution of SELECTFLUOR® (531 mg, 1.50 mmol) in anhydrous acetonitrile (4 mL) under an Ar atmosphere. The resulting mixture was then stirred at 80° C. for 12 h, then cooled to room temperature, diluted with EtOAc (2 mL), and filtered. The solvent was removed under reduced pressure and the resulting residue was chromatographed on a 24-g SiO2 pre-packed column eluting with 0:1-1:4 EtOAc/hexanes to yield 5-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester. 1H-NMR H-NMR (400 MHz, CDCl3) δ: 4.37 (q, J=7.2 Hz, 2H), 4.03 (d, J=1.0 Hz, 3H), 1.39 (t, J=7.1 Hz, 3H), 1.34 (s, 9H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09023846B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-9cc8eb99829f4846a1aa9318e1fa345f |
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| 출처 메모 | uspto-grants-2015_05 |
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