関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Trifluoromethanesulfonic acid | HCID 62406 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Iodo benzene diacetate | HCID 12217721 | — |
| 反応物 | 1-(4-Bromo-2-fluorophenyl)ethan-1-one | HCID 21938581 | — |
| 生成物 | 5-(4-Bromo-2-fluorophenyl)-2-methyloxazole | HCID 66608226 | — |
反応手順
To a suspension of iodobenzene diacetate (6.7 g) in acetonitrile (100 mL) was added dropwise trifluoromethanesulfonic acid (3.7 mL), and the mixture was stirred at room temperature for 30 min. A mixture of 1-(4-bromo-2-fluorophenyl)ethanone (6.7 g) in acetonitrile (20 mL) was added to the reaction mixture, and the mixture was heated under reflux for 2 hr. The reaction mixture was allowed to cool to room temperature, and neutralized with saturated aqueous sodium hydrogen carbonate solution, and the solvent was evaporated under reduced pressure. The residue was extracted with ethyl acetate, the extract was washed with saturated brine and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822699B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-a5e7c4b700384101bf871aa4d6851407 |
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| 出典メモ | uspto-grants-2014_09 |
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