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Acetic Anhydride → 4-Benzyloxy-2(1H)-pyridone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 4-(Benzyloxy)pyridine N-oxide | HCID 295871 | — |
| 生成物 | 4-Benzyloxy-2(1H)-pyridone | HCID 3607724 | 49% |
反応手順
4-Benzyloxypyridine 1-oxide (24.8 g, 123 mmols) was refluxed in acetic anhydride (150 mL) for 1.5 hours. Cooling the system to room temperature, the system was concentrated under reduced pressure and the resulting residue was dissolved in a mixed solvent of ethyl acetate (150 mL) and methanol (10 mL), followed by stirring at 60° C. for 2 hours. The solid formed upon cooling the system to room temperature was recovered by filtration to provide crude title compound (8.84 g). Concentrating the filtrate, additional crude title compound (4.17 g) was obtained. The combined crude product was recrystallized from a mixed solvent of methanol and ethyl acetate to provide the title compound (12.1 g, 49%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732456B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-49d140b0dab5425e960646c5242341e6 |
| 出典メモ | uspto-grants-2010_06 |