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Methyl iodide → 3-Methoxy-1-methylpyridin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3-Methoxy-2-pyridone | HCID 88731 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-Methoxy-1-methylpyridin-2-one | HCID 587024 | 89.8% |
反応手順
To a stirring reaction mixture of 3-methoxypyridine-2-one (0.2 g, 1.6 mmol) and KOH (0.18 g, 3.2 mmol) in methanol was added MeI (0.68 g, 4.8 mmol) dropwise in condenser equipped round bottom flask. After overnight stirring at room temperature revealed quantitative formation of product. Reaction mixture was then diluted with water (35 mL) and CHCl3 (40 mL). Organic layer was washed with water (1×35 mL), brine (1×30 mL) and dried over Na2SO4 and solvent was evaporated in vacua to yield pure 141a (0.20 g, 89%) as a colorless oil. 1H NMR (400 MHz, CDCl3) δ 6.66 (m, 1H), 6.35 (d, J=7.4 Hz, 1H), 5.83 (t, J=7.1 Hz, 1H), 3.52 (s, 3H), 3.28 (s, 3H). 13C NMR (100 MHz, CDCl3) δ 158.01, 149.56, 128.81, 111.91, 104.31, 55.44, 37.10.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871728B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-d82537a4ccee495a8f1d49727f011359 |
| 出典メモ | uspto-grants-2014_10 |