참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Biphenyl-2-boronic acid | HCID 4589187 | — |
| 반응물 | 2,7-Dibromo-9,9-dimethylfluorene | HCID 12123876 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 2-(biphenyl-2-yl)-7-bromo-9,9-dimethyl-9H-fluorene | HCID 57622876 | 63% |
반응 단계
A mixture of 35.2 g (100 mmol) of 2,7-dibromo-9,9-dimethyl-9H-fluorene, 21.8 g (110 mmol) of biphenyl-2-ylboronic acid, 2.31 g (2 mmol) of Tetrakis(triphenylphosphine)palladium, 75 ml of 2M Na2CO3, 150 ml of EtOH and 300 ml toluene was degassed and placed under nitrogen, and then heated at 100° C. for 12 h. After finishing the reaction. The mixture was allowed to cool to room temperature. The organic layer was extracted with ethyl acetate and water, dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica (hexane-dichloromethane) to give product (26.8 g, 63.0 mmol, 63%) as a white solid. 1H NMR (CDCl3, 400 MHz): δ 7.61 (d, J=7.8 Hz, 1H), 7.55˜7.53 (m, 2H), 7.49˜7.42 (m, 5H), 7.29 (d, J=8.0 Hz, 1H), 7.20˜7.14 (m, 5H), 6.98 (s, 1H), 1.21 (s, 6H)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09040174B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-524a22c7898446ee9df4c0ed23cf42d6 |
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| 출처 메모 | uspto-grants-2015_05 |
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