関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromodibenzothiophene | HCID 458352 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 反応物 | 9-Phenyl-9H,9'H-[3,3']bicarbazolyl | HCID 59306629 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 触媒 | 2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl | HCID 11269872 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | HCID 58479599 | HCID 58479599 | 76% |
反応手順
A mixture of 4-bromodibenzo[b,d]thiophene (2.061 g, 7.83 mmol), 9-phenyl-9H,9′H-3,3′-bicarbazole (2 g, 4.90 mmol), and sodium t-butoxide (1.412 g, 14.69 mmol) in 200 mL of xylene was bubbled with N2 for 20 min. Pd2(dba)3 (0.045 g, 0.049 mmol) and dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (0.080 g, 0.196 mmol) were added and bubbled with nitrogen for another 20 min, then the mixture was heated to reflux under N2 for 24 h. The mixture was cooled and filtered through Celite. After solvent evaporation, the residue was coated on Celite and purified by column chromatography using 2:3 dichloromethane and hexanes as solvent. 9-(dibenzo[b,d]thiophen-4-yl)-9′-phenyl-9H,9′H-3,3′-bicarbazole (2.2 g. 3.72 mmol, 76% yield) was obtained. The product was further purified by recrystallization with dichloromethane and hexane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08227801B2 |
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| 出典データセット | uspto-grants-2012_07 |
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| ORD ID | ord-8e04e65685da42ab98a212a8c41ac2cc |
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| 出典メモ | uspto-grants-2012_07 |
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