関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Acetyl-4-fluorophenol | HCID 95992 | — |
| 反応物 | 4-Chloro-6,7-dimethoxyquinoline | HCID 459610 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 生成物 | 1-{2-[(6,7-Dimethoxy-4-quinolyl)oxy]-5-fluorophenyl}-1-ethanone | HCID 24879101 | 72% |
反応手順
4-Chloro-6,7-dimethoxyquinoline (58.2 mg), 5-fluoro-2-hydroxyacetophenone (409 mg), and 4-dimethylaminopyridine (317 mg) were suspended in o-dichlorobenzene (5 ml), and the suspension was stirred at 160° C. for 8 hr. The reaction solution was cooled to room temperature, and the solvent was then removed therefrom by distillation under the reduced pressure. Chloroform was added to the residue, and the organic layer was washed with a 1 N aqueous potassium hydroxide solution and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography using chloroform and by thin layer chromatography using acetone-hexane to give the title compound (63.5 mg, yield 72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560558B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-292ee15e054a4432bd8fe045a6d76269 |
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| 出典メモ | uspto-grants-2009_07 |
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