참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,5-Difluorobenzonitrile | HCID 123558 | — |
| 반응물 | 1h-1,2,4-Triazole sodium salt | HCID 45489822 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-fluoro-2-(1H-1,2,4-triazol-1-yl)benzonitrile | HCID 21866254 | 49% |
반응 단계
A suspension of 2,5-diflurobenzonitrile (4.5 g, 32.35 mmol) and 1,2,4-triazole sodium salt (3.6 g, 40 mmol) in dimethylformamide (40 mL) was heated at 80° C. for 15 h. The reaction mixture was then cooled, diluted with CH2Cl2 (200 mL), washed with water (3×30 mL) and brine (30 mL), then dried (Na2SO4), filtered and concentrated to give a white solid which was purified by flash column chromatography (SiO2) using 1:1 to 3:1 ethyl acetate/Hexanes to afford the title compound (2.98 g, 49% yield) as a white powder. 1H NMR (500 MHz, CDCl3) δ: 8.70 (1H, s), 8.18 (1H, s), 7.76 (1H, dd, J=9.0, 4.8 Hz), 7.55 (1H, dd, J=7.3, 2.8 Hz), 7.51–7.47 (1H, m). LCMS (M+H) calcd for C9H6FN4: 189.17. found: 189.10.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07157447B2 |
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| 출처 데이터셋 | uspto-grants-2007_01 |
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| ORD ID | ord-680d9b7e444f48a9a3331970ca20fee7 |
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| 출처 메모 | uspto-grants-2007_01 |
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