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Ethanol → 1-(1,2,2a,3,4,5-Hexahydroacenaphthylen-1-yl)piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Ethyl-1-methyl-4-oxopiperidin-1-ium iodide | HCID 11097568 | — |
| 反応物 | 1,2,2a,3,4,5-Hexahydroacenaphthylen-1-amine | HCID 63821374 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(1,2,2a,3,4,5-Hexahydroacenaphthylen-1-yl)piperidin-4-one | HCID 68706671 | 14% |
反応手順
To a mixture of 1,2,2a,3,4,5-hexahydroacenaphthylen-1-ylamine, potassium carbonate (3.89 g) and ethanol (60 ml) was added 1-ethyl-1-methyl-4-oxopiperidinium iodide (8.36 g) dissolved in water (15 ml), and the mixture was heated under reflux for 2 hr. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over magnesium sulfate, and concentrated. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 1-(1,2,2a,3,4,5-hexahydroacenaphthylen-1-yl)piperidin-4-one (1.01 g, 14%) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877779B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-27bbfc698e0847b9a4e7cddf3b391f15 |
| 出典メモ | uspto-grants-2014_11 |