関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 3-chloro-2-oxopiperidine-3-carboxylate | HCID 568505 | — |
| 反応物 | 3,4,5-Trifluorophenol | HCID 2777943 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | Ethyl 2-oxo-3-(3,4,5-trifluorophenoxy)piperidine-3-carboxylate | HCID 66607659 | 79.8% |
反応手順
To a mixture of 3,4,5-trifluorophenol (14.4 g) and potassium carbonate (40.3 g) in DMF (200 mL) was added ethyl 3-chloro-2-oxopiperidine-3-carboxylate (20 g), and the mixture was stirred at 100° C. for 1 hr. To the reaction mixture were added water (200 mL) and saturated brine (200 mL) at 0° C., and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution (200 mL), water (200 mL) and saturated brine (200 mL×2), 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 (24.61 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-106c5625101a4a4f9382f4921d49f5df |
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| 出典メモ | uspto-grants-2014_09 |
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