関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 反応物 | Indolo[2,3-a]carbazole | HCID 21882147 | — |
| 反応物 | 4-Carbazolylbromobenzene | HCID 23143955 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 11-(4-Carbazolylphenyl)indolo[2,3-a]carbazole | HCID 66937598 | 47% |
反応手順
In a 100-ml three-necked flask were placed 0.21 g (0.94 mmole) of palladium(II) acetate, 20 ml of xylene, and 0.76 g (3.76 mmoles) of tri-tert-butylphosphine and the mixture was heated at 60° C. with stirring for 30 minutes. The resulting solution was sent into a solution that had been prepared by dissolving 4.61 g (0.0180 mole) of indolo[2,3-a]carbazole, 5.8 g (0.018 mole) of 4-carbazolylbromobenzene, and 7.7 g (0.080 mole) of sodium tert-butoxide in 180 ml of xylene and heated at 60° C. in a stream of nitrogen and the combined solution was heated up to 130° C. and kept at this temperature for 5 hours with stirring. The solution was cooled to room temperature, 200 ml of water was added, and the organic layer was separated and concentrated under reduced pressure to give a crude product. The crude product was purified by crystallization from dichloromethane and ethanol, the solvent was distilled off under reduced pressure, and 4.2 g (0.0084 mole, 47% yield) of 11-(4-carbazolylphenyl)indolo[2,3-a]carbazole was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08062769B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-6858f3c062f24685a3d9f60c0b864aed |
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| 出典メモ | uspto-grants-2011_11 |
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