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Selenium Dioxide → 3-Hydroxy-6-methylpyridine-2-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Selenium Dioxide | HCID 24007 | — |
| 反応物 | 3-Hydroxy-2-hydroxymethyl-6-methylpyridine | HCID 135128 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Hydroxy-6-methylpyridine-2-carbaldehyde | HCID 12421986 | 57.3% |
反応手順
3-Hydroxy-6-methyl-2-pyridine methanol (20.0 g, 0.14 mol) and selenium dioxide(8.0 g, 72 mmol) were dissolved in 140 mL of 1,4-dioxane and 280 mL of absolute ethanol. The resulting mixture was heated at 80°-85° C. for 12 h. The selenium precipitate was removed by filtration and the filtrate was concentrated to dryness in vacuo. The dark red residue was sublimed at 90° C. and 14 mmHg for 6 h to obtain 11.0 g (56%) of pure product, m.p. 101°-102° C.; 1H NMR (CDCl3) δ: 10.50 (br s, 1H), 10.03 (s, 1H), 7.27 (s, 2H); 2.53 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726314 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-0570825de3de42f284cb61b4bb3699df |
| 出典メモ | uspto-grants-1998_03 |