反应详情

温度

120 °C

4,4′-dimethyldiphenylamine (0.99 g, 5.0 mmol), KOH (2.52 g, 45.0 mmol), CuCl (99 mg, 1.0 mmol) and 1,10-phenanthroline (180 mg, 1.0 mmol) were charged in a two-necked bottle. The bottle was deoxygenated and purged with nitrogen, and added dried toluene (12 mL) and iodobenzene (0.67 ml, 6.0 mmol). The reaction was heated to 120° C., and stirred for 12 hours. The resulting was filtered to remove metal and then concentrated under reduced pressure and the residue was purified by column chromatography (hexanes/CH2Cl2=1/1) to afford G (916 g, 67%) as white solid.

1. customThe bottle was deoxygenated
2. custompurged with nitrogen
3. filtrationThe resulting was filtered
4. customto remove metal
5. concentrationconcentrated under reduced pressure
6. customthe residue was purified by column chromatography (hexanes/CH2Cl2=1/1)
7. customto afford G (916 g, 67%) as white solid