関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Phenyl-2-propen-1-one | HCID 13028 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 1,3-Dimethyl-4-piperidone | HCID 107311 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,3-Dimethyl-3-(3-oxo-3-phenyl-propyl)-piperidin-4-one | HCID 67357110 | 10.8% |
反応手順
To a stirred solution of 1,3-dimethyl-piperidin-4-one (0.1 g, 0.787 mmol) in mixture of 1,4 dioxane (2 mL) and water (0.1 mL) was added crushed KOH (44 mg, 0.787 mmol). The reaction mixture was stirred at 25° C. for 10 min. To this was added 1-phenylprop-2-en-1-one (103 mg, 0.787 mmol) dropwise. The reaction mixture was stirred at 25° C. for 2 h. The reaction mixture was concentrated under reduced pressure and the residue was diluted with water (10 mL) and EtOAc (20 mL), the organic layer was separated, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting crude product was purified by column chromatography on neutral alumina (eluted with EtOAc:Hexanes, 1:99) to afford 1,3-dimethyl-3-(3-oxo-3-phenyl-propyl)-piperidin-4-one as an oil (22 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09040519B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-0c551d20fef6440ca1f200327530665c |
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| 出典メモ | uspto-grants-2015_05 |
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