반응 #479700

반응 방정식

4,4′-Dibromo-2-amino-1,1′-biphenyl

iodobenzene

potassium hydroxide

1,10-phenanthroline

→

white crystals

4,4′-DIBROMO-2-DIPHENYLAMINO-1,1′-BIPHENYL

용매

toluene

toluene

반응 조건

후처리

1. 1
   온도at reflux for 15 hours
2. 2
   기타The dark reaction mixture
3. 3
   세척The toluene solution was washed with DI water
4. 4
   건조dried with magnesium sulfate
5. 5
   기타evaporated
6. 6
   기타The dark residue obtained
7. 7
   기타was recrystallized trice from hexane/toluene (4:1 in volume)

실험 절차

4,4′-Dibromo-2-amino-1,1′-biphenyl (16.35 g, prepared according to Libman and Slack (1951) J. Chem. Soc., p. 2588), iodobenzene (26.52 g, 0.13 mol), flake potassium hydroxide (22.4 g, 0.35 mol), 1,10-phenanthroline (0.45 g), copper (I) chloride (0.25 g), and toluene (30 ml) were charged into a flask and stirred at reflux for 15 hours. The dark reaction mixture was cooled to room temperature and diluted with 200 ml of toluene. The toluene solution was washed with DI water, dried with magnesium sulfate, and evaporated. The dark residue obtained was recrystallized trice from hexane/toluene (4:1 in volume) to yield 10 grams of white crystals to yield the desired monomer. 1H NMR (CDCl3): δ=6.8-7.5, multiple peaks.

출처