関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 5-Methoxy-4-methylindole | HCID 3296242 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-methyl-1H-indol-5-ol | HCID 21691244 | — |
反応手順
5-Methoxy-4-methyl-1H-indole (10 g, 62.0 mmol) is dissolved in DCM (400 mL) and cooled to 0° C. BBr3 (155 mL, 155 mmol) is added dropwise over 1 hour and the black mixture is allowed to warm to room temperature overnight (17 hours). The reaction is poured over a mixture of ice and sodium bicarbonate (aq) solution and extracted with ethyl acetate (1.5 L) and concentrated to a black oil. The oil is absorbed onto silica and separated via FCC (0-50% ethyl acetate:heptanes) to obtain the title compound as a solid. MS (ESI) m/z 148.23 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541432B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-191d2f4148c141ae8c91cc9f7f567cfc |
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| 出典メモ | uspto-grants-2013_09 |
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