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Ethanol → Ethyl 5-hydroxy-1H-indole-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 5-Hydroxyindole-2-carboxylic acid | HCID 88958 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | Ethyl 5-hydroxy-1H-indole-2-carboxylate | HCID 90677 | 88% |
反応手順
5-Hydroxy-1H-2-indolecarboxylic acid (328 mg) was dissolved in ethanol (10 ml) to prepare a solution. Concentrated sulfuric acid was added to the solution, and the mixture was heated under reflux for 3 hr. The reaction solution was cooled to room temperature, an aqueous sodium hydrogencarbonate solution was then added thereto, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with saturated brine and was dried over anhydrous magnesium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography on silica gel using ethyl acetate-hexane to give ethyl 5-hydroxy-1H-2-indolecarboxylate (336 mg, yield 88%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560558B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-168586367db641459e78c5c99289aa25 |
| 出典メモ | uspto-grants-2009_07 |