関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-2,2-difluoroacetophenone | HCID 238296 | — |
| 反応物 | 6-Fluoro-8-hydroxy-2-methylquinoline | HCID 66781517 | — |
| 生成物 | HCID 70984374 | HCID 70984374 | — |
反応手順
To a mixture of 6-fluoro-2-methylquinolin-8-ol (0.15 g, 0.85 mmol) and potassium carbonate (4.2 g, 30 mmol) in acetonitrile (3.4 mL, 0.85 mmol) and water (3.4 mL, 0.85 mmol) was added 2-chloro-2,2-difluoroacetophenone (0.62 mL, 4.2 mmol). The vessel was sealed and the mixture was heated at 80° C. for 4 hours. The cooled reaction mixture was extracted with diethyl ether (2×30 mL), and the combined organic extracts were dried over magnesium sulfate, filtered and concentrated under reduced pressure at ambient temperature The resulting residue was purified by reverse phase chromatography on a C18 column (0-100% acetonitrile/water). Aqueous fractions containing the product were combined and extracted with diethyl ether (2×100 mL). The combined organic extracts were dried over magnesium sulfate, filtered and concentrated under reduced pressure at ambient temperature providing the title compound. Presence of water was noted and the material taken on as is assuming theoretical yield obtained (0.19 g, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889704B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-75c94b7ae1fc4b6fba7882526e3a2fab |
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| 出典メモ | uspto-grants-2014_11 |
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