Реакция #11841

Уравнение реакции

4,4′-Dibromo-2-amino-1,1′-biphenyl

iodobenzene

potassium hydroxide

1,10-phenanthroline

→

white crystals

4,4′-Dibromo-2-Diphenylamino-1,1′-Biphenyl

Растворители

toluene

toluene

Условия реакции

Обработка

1. 1
   Температураat reflux for 15 hours
2. 2
   ДругоеThe dark reaction mixture
3. 3
   ПромывкаThe toluene solution was washed with DI water
4. 4
   Сушкаdried with magnesium sulfate
5. 5
   Другоеevaporated
6. 6
   ДругоеThe dark residue obtained
7. 7
   Другоеwas recrystallized trice from hexane/toluene (4:1 volume)

Методика

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 volume) to yield 10 grams of white crystals to yield the desired monomer. 1H NMR (CDCl3): δ=6.8–7.5, multiple peaks.

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