関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(3-Hydroxypropyl)-2-mercapto-5-hydroxymethylimidazole | HCID 178520822 | — |
| 触媒 | Tungstic acid | HCID 1152 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(3-Hydroxypropyl)-5-hydroxymethylimidazole | HCID 22988642 | 95.6% |
反応手順
1-(3-Hydroxypropyl)-2-mercapto-5-hydroxymethylimidazole(5.0 g, 23.1 mmol) and tungstic acid(H2WO4, 58 mg, 1 mol %) were mixed in 25 ml of methanol and 25 ml of distilled water. The mixture was warmed to 40° C. and 3.6 g of 30% hydrogen peroxide was added dropwise thereto. The whole mixture was stirred for 15 minutes and cooled and then, neutralized with 1 N sodium hydroxide solution. The resulting mixture was extracted twice with 25 ml of n-butanol and the solvent was distilled under reduced pressure to give 3.45 g(Yield 80.7%) of the title compound. 1H NMR (500 MHz, CDCl3) δ 7.46 (1H, s), 6.91 (1H, s), 4.61 (2H, s), 4.15 (2H, t, J=7 Hz), 3.52 (2H, t, J=7 Hz), 2.01 (2H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06630593B1 |
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| 出典データセット | uspto-grants-2003_10 |
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| ORD ID | ord-8e9566bc6dcb4904b94cfead5e15585a |
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| 出典メモ | uspto-grants-2003_10 |
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