참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 반응물 | Indolo[2,3-a]carbazole | HCID 21882147 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 반응물 | 3-Carbazolylbromobenzene | HCID 66937316 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | 11-(4-Carbazolylphenyl)indolo[2,3-a]carbazole | HCID 66937598 | 47% |
반응 단계
In a 100-ml three-necked flask that had been deaerated and filled with nitrogen was placed a solution of 0.21 g (0.94 millimole) of palladium(II) acetate, 0.76 g (3.8 millimoles) of tri-tert-butylphosphine was added, and the mixture was heated at 60° C. with stirring for 30 minutes. The resulting solution was transferred under nitrogen flow to a solution heated at 60° C. of 4.6 g (18.0 millimoles) of indolo[2,3-a]carbazole, 5.8 g (18.0 millimoles) of 3-carbazolylbromobenzene, and 7.7 g (80.0 millimoles) of sodium tert-butoxide in 180 ml of xylene. The solution was then heated to 130° C., and heated with stirring at this temperature for 5 hours. The solution was cooled to room temperature and 200 ml of water was added. The mixture was subjected to oil-water separation, and the organic layer was concentrated under reduced pressure to give a crude product. The crude product was purified by crystallization from dichloromethane and ethanol, the solvent was stripped off under reduced pressure, and 4.2 g (8.4 millimoles, 47% yield) of 11-(4-carbazolylphenyl)indolo[2,3-a]carbazole was obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08758904B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-a9948952bf76433eafe4ea80146ae1c3 |
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| 출처 메모 | uspto-grants-2014_06 |
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