反応 #11841

反応方程式

4,4′-Dibromo-2-amino-1,1′-biphenyl

iodobenzene

potassium hydroxide

1,10-phenanthroline

→

white crystals

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

溶媒

toluene

toluene

反応条件

後処理

1. 1
   温度at reflux for 15 hours
2. 2
   その他The dark reaction mixture
3. 3
   洗浄The toluene solution was washed with DI water
4. 4
   乾燥dried with magnesium sulfate
5. 5
   その他evaporated
6. 6
   その他The dark residue obtained
7. 7
   その他was recrystallized trice from hexane/toluene (4:1 volume)

実験手順

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.

出典