関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 5-Hydroxyindole | HCID 16054 | — |
| 反応物 | (4-Chloropyridin-2-yl)methanol | HCID 2763167 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | (4-(1H-indol-5-yloxy)pyridin-2-yl)methanol | HCID 59394421 | — |
反応手順
To a solution of (4-chloropyridin-2-yl)methanol (384 mg, 2.67 mmol) in DMF (12 mL) is added 1H-indol-5-ol (534 mg, 4.01 mmol), and cesium carbonate (1307 mg, 4.01 mmol). The reaction is sealed and heated to 160° C. via microwave irradiation for 30 min. The reaction mixture is then cooled to room temperature and diluted brine and DCM. The resulting layers are separated and the aqueous layer is extracted three additional times with DCM. The organic layers are combined dried over anhydrous Na2SO4, filtered, and concentrated. The resulting residue is purified via FCC (0-100% EtOAc/heptane) to give the title compound. MS (ESI) m/z 241.2 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08492393B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-107983992ccc44b7848065f643ca1a1f |
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| 出典メモ | uspto-grants-2013_07 |
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