反应详情

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.

1. customA 100 ml four-neck flask provided with a thermometer, stirrer
2. temperaturereflux tube
3. additionnitrogen-introducing tube
4. stirringthe result stirred at room temperature
5. dissolutionuntil dissolving
6. temperatureAn oil bath was heated to 60° C.
7. filtrationThe reaction solution was filtered
8. washrinsed away with a small amount of methanol
9. stirringThe filtered material was stirred in 30 ml of methanol for 30 minutes
10. filtrationfiltered
11. customThe obtained residue was dried at 60° C. under reduced pressure