반응 #505213

반응 방정식

triphenylene

1,3-diiodobenzene

potassium carbonate

toluene

→

1,3-bis(triphenylen-2-yl)benzene

용매

water

반응 조건

후처리

1. 1
   기타The system was purged by nitrogen for 10 min
2. 2
   workup.ADDITIONbefore adding 0.05 g of Pd(PPh3)4
3. 3
   workup.ADDITIONto the mixture was added 200 mL of methanol
4. 4
   여과The precipitate was collected by filtration
5. 5
   세척The solid was washed with copious amount of methanol
6. 6
   기타The solid was then recrystallized from 80 ml of xylenes
7. 7
   기타Final purification of the product
8. 8
   기타at 250° C
9. 9
   기타0.35 g product was collected as white needle crystals

실험 절차

1.23 g (3.5 mmol) of the triphenylene moronic ester from the previous step, 0.5 g (1.5 mmol) of 1,3-diiodobenzene, 1.0 g (7.5 mmol) of potassium carbonate, 30 mL of toluene, and 10 mL of water was mixed in a 250 mL three-neck flask. The system was purged by nitrogen for 10 min before adding 0.05 g of Pd(PPh3)4. The mixture was then heated up to 87° C. with vigorous stirring. After 24 hr, to the mixture was added 200 mL of methanol. The precipitate was collected by filtration. The solid was washed with copious amount of methanol, then hexanes. The solid was then recrystallized from 80 ml of xylenes. Final purification of the product involved subliming the material at 250° C. 0.35 g product was collected as white needle crystals.

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