関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2,4-Dimethoxy-1-nitrobenzene | HCID 78633 | — |
| 反応物 | 3,5-Dichloro-1-fluoropyridinium triflate | HCID 2724578 | — |
| 溶媒 | 1,1,1,2-Tetrachloroethane | HCID 12418 | — |
| 生成物 | 2,4-Dimethoxy-5-fluoronitrobenzene | HCID 2758414 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06271236B1 |
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| 出典データセット | uspto-grants-2001_08 |
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| ORD ID | ord-beefefe3761740c4b3b00c80aa88b061 |
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| 出典メモ | uspto-grants-2001_08 |
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