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Diisopropyl Ether → phenylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Bromothieno[2,3-b][1,5]benzoxazepin-4(5H)-one | HCID 18422193 | — |
| 反応物 | Phenylborate | HCID 19793864 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Sodium Carbonate | HCID 10340 | — |
| 生成物 | phenylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one | HCID 18422186 | 83.8% |
反応手順
2-Bromothieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.0 g) was dissolved in 2M sodium carbonate (8 ml)-toluene (8 ml)-ethanol (8 ml) and phenyl borate (620 mg) and tetrakstriphenylphosphine palladium (390 mg) were added. The mixture was stirred under reflux with heating for 80 minutes. The reaction system was cooled to room temperature and diisopropyl ether and ethyl acetate were added. The precipitated crystals were collected by filtration and the obtained crystals were washed with ethyl acetate and water to give phenylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (830 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06271225B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-b04ddccd5c894e45a90bb6cdb81f3a2a |
| 出典メモ | uspto-grants-2001_08 |