関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Carbethoxy-2-piperidone | HCID 97773 | — |
| 反応物 | 4-(Bromomethyl)-1,2-difluorobenzene | HCID 581436 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Ammonium Chloride | HCID 25517 | — |
| 生成物 | Ethyl 3-(3,4-difluorobenzyl)-2-oxopiperidine-3-carboxylate | HCID 66607767 | — |
反応手順
Under a nitrogen atmosphere, to a mixture of ethyl 2-oxopiperidine-3-carboxylate (2.0 g) in DMF (20 mL) was added sodium hydride (60%, 0.47 g) at 0° C., and the mixture was stirred at 0° C. for 30 min. 4-(Bromomethyl)-1,2-difluorobenzene (1.50 mL) was added to the reaction mixture, and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and saturated aqueous ammonium chloride solution, the mixture 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 (2.82 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-6984390e460d42cfaf5e95d0ceef91d0 |
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| 出典メモ | uspto-grants-2014_09 |
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