참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2,4-Dimethoxy-1-nitrobenzene | HCID 78633 | — |
| 반응물 | 3,5-Dichloro-1-fluoropyridinium triflate | HCID 2724578 | — |
| 용매 | 1,1,1,2-Tetrachloroethane | HCID 12418 | — |
| 생성물 | 2,4-Dimethoxy-5-fluoronitrobenzene | HCID 2758414 | — |
반응 단계
To a solution of 2,4-dimethoxy-nitrobenzene (1.0 g) in tetrachloroethane (10 mL) is added 3,5-dichloro-1-fluoro-pyridinium triflate (85%, 5.07 g) and the mixture is heated to 120° C. for 5 hours. Additional 3,5-dichloro-1-fluoro-pyridinium triflate (85%, 0.25 g) is added and heating is continued for 1 hour. The solution is then cooled to room temperature and passed over a column of silica gel (hexanes followed by 30% ethyl acetate in hexanes is used as the eluant). Product containing fractions are combined, evaporated under reduced pressure, and the residue is crystallized from hexanes to provide the desired product as a tan solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06271236B1 |
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| 출처 데이터셋 | uspto-grants-2001_08 |
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| ORD ID | ord-beefefe3761740c4b3b00c80aa88b061 |
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| 출처 메모 | uspto-grants-2001_08 |
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