関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | 1-(p-Hydroxyphenyl)imidazole | HCID 82315 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Imidazol-1-yl)-2-iodophenol | HCID 22274493 | 14% |
反応手順
4-(Imidazol-1-yl)phenol (500 mg) was dissolved in water (6 ml), methanol (18 ml), and dichloromethane (6 ml) to prepare a solution. Iodine (1.58 g) was added to the solution, and the mixture was stirred at room temperature for 8 days. An aqueous sodium thiosulfate solution and methanol were added to the reaction solution, and the mixture was stirred and was then concentrated. The concentrate was extracted with chloroform, and the chloroform layer was then washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give 4-(imidazol-1-yl)-2-iodophenol (123 mg, yield 14%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560558B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-6443b95ed90b4833a2ab64a8d940ff33 |
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| 出典メモ | uspto-grants-2009_07 |
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