関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tert-Butylamine | HCID 6385 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-Ethyl-1-methyl-4-oxopiperidin-1-ium iodide | HCID 11097568 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-tert-Butyl-4-piperidone | HCID 73840 | 60.9% |
反応手順
To a solution of t-butylamine (78.2 ml, 0.74 mol) in toluene (400 ml) was added a solution of 1-ethyl-1-methyl-4-oxopiperidinium iodide (40 g, 0.148 mol) and sodium bicarbonate (1.245 g, 0.014 mol) in water (60 ml). The reaction mixture was heated at 78° C. for 6 hours and then allowed to cool to ambient temperature. The layers were separated and the aqueous layer was washed with EtOAc. The organics were combined and washed with brine, dried (MgSO4), filtered and reduced in vacuo to yield 1-tert-butyl-4-oxopiperidine (14 g) (LC/MS: Rt 0.39, [M+H]+ 156).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745638B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-16ead13fb039460189a4c95fd97d5f44 |
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| 出典メモ | uspto-grants-2010_06 |
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