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m-Chloroperbenzoic acid → 2-Chloro-5-methoxy-3-methylpyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 2-Chloro-5-methoxy-3-methylpyridine | HCID 12852016 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-5-methoxy-3-methylpyridine 1-oxide | HCID 86717815 | — |
反応手順
3-Chloroperoxybenzoic acid (70%, 695 mg, 2.82 mmol) was added to a solution of 2-chloro-5-methoxy-3-methylpyridine (370 mg, 2.35 mmol) in dichloromethane (10 mL). After stirring for 18 hours at room temperature, the reaction mixture was concentrated in vacuo and purified via silica gel chromatography (Gradient: 0% to 10% methanol in ethyl acetate) to afford the product as a white solid. Yield: 370 mg, 2.13 mmol, 91%. 1H NMR (400 MHz, CD3OD) δ 8.14 (d, J=2.5 Hz, 1H), 7.23 (d, J=2.3 Hz, 1H), 3.88 (s, 3H), 2.44 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822494B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-04113bd597ee43be87c8b0ace7ac50f1 |
| 出典メモ | uspto-grants-2014_09 |