関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | 2,7-Dibromocarbazole | HCID 11151503 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,7-Dibromo-9-phenylcarbazole | HCID 22392517 | 78% |
反応手順
A mixture of 32.5 g (100 mmole) 2,7-dibromo-9H-carbazole, 20.4 g (100 mmole) iodobenzene, 9.5 g (150 mmole) of copper powder, 27.6 g (200 mmole) of potassium carbonate, and 600 ml dimethylformamide were heated at 130° C. under nitrogen overnight, then cooled to room temperature, the solution was filtered. The filtrate was extracted three times with dichloromethane and water, dried with anhydrous magnesium sulfate, the solvent was evaporated in vacuum. The residue was purified by column chromatography on silica(hexane-dichloromethane) afforded a white solid (31.3 g, 78 mmol, 78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09166177B2 |
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| 出典データセット | uspto-grants-2015_10 |
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| ORD ID | ord-a64844fa08ed4a9a98c984928b777f73 |
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| 出典メモ | uspto-grants-2015_10 |
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