関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Hydroxy-2(1H)-pyridinone | HCID 54696004 | — |
| 反応物 | Benzyl 4-((methanesulfonyl)oxy)piperidine-1-carboxylate | HCID 58303455 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzyl 4-(2-oxo-1,2-dihydropyridin-4-yloxy)piperidine-1-carboxylate | HCID 67366192 | 37.2% |
反応手順
A stirring suspension of benzyl 4-(methylsulfonyloxy)piperidine-1-carboxylate (1.97 g, 6.30 mmol), 4-hydroxypyridin-2(1H)-one (0.50 g, 4.5 mmol, Aldrich), potassium carbonate (1.43 g, 10.6 mmol, EMD) and DMF (25 mL) was heated at 140° C. for 2.5 h and then cooled to room temperature. The resulting mixture was diluted with H2O and extracted with EtOAc (2×). The organic layers were combined and washed with brine, dried over Na2SO4 and concentrated in vacuo to a light yellow oil. The oil was purified by flash chromatography (SiO2, 0 to 10% MeOH in CH2Cl2) to yield 550 mg of desired product as a white solid. MS (ESI) 329 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08003796B2 |
|---|
| 出典データセット | uspto-grants-2011_08 |
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| ORD ID | ord-31c2ef5221a9487792f750d6cf7476e1 |
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| 出典メモ | uspto-grants-2011_08 |
|---|
