関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Biphenyl-2-boronic acid | HCID 4589187 | — |
| 反応物 | 2,7-Dibromo-9,9-dimethylfluorene | HCID 12123876 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(biphenyl-2-yl)-7-bromo-9,9-dimethyl-9H-fluorene | HCID 57622876 | 63% |
反応手順
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)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09040174B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-524a22c7898446ee9df4c0ed23cf42d6 |
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| 出典メモ | uspto-grants-2015_05 |
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