関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl isonicotinate | HCID 15291 | — |
| 反応物 | 4-Chloropyridine hydrochloride | HCID 81852 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(Pyridin-4-yl)piperidine-4-carboxylic acid | HCID 1268289 | 78.7% |
反応手順
4-Chloropyridine hydrochloride (9.55 g) and triethylamine (26.0 ml) are dissolved in ethanol (10 ml) and water (30 ml), and thereto is added ethyl isonicotinate (10.00 g). The reaction solution is then heated at 150° C. for 96 hours in a sealed tube. After allowing to cool, ethanol is added to the reaction solution and the insoluble materials are removed by filtration. The filtrate is concentrated under reduced pressure, and the resulting residue is suspended in chloroform. The precipitates are collected by filtration and recrystallized from water/N,N-dimethylformamide to give the title compound (10.34 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737161B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-cc361223dfd14718a49e0b82a2f7cfe8 |
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| 出典メモ | uspto-grants-2010_06 |
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