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Hydrogen Peroxide → 2,4-Dimethylpyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 2,4-Dimethylpyridine | HCID 7936 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2,4-Dimethylpyridine 1-oxide | HCID 70733 | 98% |
反応手順
2,4-Dimethylpyridine (40 g, 0.37 mol) was stirred with 30% hydrogen peroxide (170 ml) in glacial acetic acid (400 ml) in an oil bath (80-90° C.) for 24 hr. After cooling to room temperature, the mixture was evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, 1) ether, 2) methanol:chloroform (8:92)) to afford 45 g (98%) of 2,4-dimethyl-pyridine 1-oxide as an oil. 1H NMR (200 MHz, DMSO-d6) δ 2.02 (3H, s), 2.18 (3H, s), 6.69 (1H, d, J=6.5 Hz), 6.82 (1H, s), 7.84 (1H, d, J=6.5 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08106064B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-3b557427a55c4199b11e2115640f5a1c |
| 出典メモ | uspto-grants-2012_01 |