関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2'-Dimethylbiphenyl | HCID 11797 | — |
| 反応物 | 1-Bromoadamantane | HCID 79106 | — |
| 触媒 | Iron chloride (FeCl3) | HCID 24380 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | 2,2'-Dimethyl-5,5'-bis(1-adamantyl)biphenyl | HCID 86641950 | 48.2% |
反応手順
A 100 ml four-neck flask provided with a thermometer, stirrer, reflux tube, and nitrogen-introducing tube was charged with 2,2′-dimethylbiphenyl 14.7 g (80.55 mmol), 1-bromo-adamantane 34.7 g (161.1 mmol), and nitromethane 200 ml and the mixture stirred under a nitrogen flow at room temperature. Iron (III) chloride 1.31 g (8.07 mmol) was added and the result stirred at room temperature until dissolving. An oil bath was heated to 60° C., then the stirring was continued at that temperature for 4 hours. The reaction solution was filtered and rinsed away with a small amount of methanol. The filtered material was stirred in 30 ml of methanol for 30 minutes, then filtered. The obtained residue was dried at 60° C. under reduced pressure to obtain 2,2′-dimethyl-5,5′-bis(1-adamantyl)biphenyl white powder 17.5 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530596B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-5cb30b4366f44281b496e7a76d17fed4 |
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| 出典メモ | uspto-grants-2013_09 |
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