반응 #69566

반응 방정식

2,2′-dimethylbiphenyl

1-bromo-adamantane

→

2,2′-dimethyl-5,5′-bis(1-adamantyl)biphenyl

수율 48.2%

용매

nitromethane

반응 조건

후처리

1. 1
   기타A 100 ml four-neck flask provided with a thermometer, stirrer
2. 2
   온도reflux tube
3. 3
   workup.ADDITIONnitrogen-introducing tube
4. 4
   workup.STIRRINGthe result stirred at room temperature
5. 5
   workup.DISSOLUTIONuntil dissolving
6. 6
   온도An oil bath was heated to 60° C.
7. 7
   여과The reaction solution was filtered
8. 8
   세척rinsed away with a small amount of methanol
9. 9
   workup.STIRRINGThe filtered material was stirred in 30 ml of methanol for 30 minutes
10. 10
    여과filtered
11. 11
    기타The obtained residue was dried at 60° C. under reduced pressure

실험 절차

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.

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