反应详情

A mixture of 4-phenylazophenol (9.9 g; 50 mmol), iodomethane (7.1 g; 50 mmol), potassium carbonate (6.9 g; 50 mmol), and acetone (100 ml) was refluxed 48 h. After evaporating off the solvent, the residue was dissolved in water (25 ml), diethyl ether (50 ml) and THF (30 ml). The aqueous layer was extracted with ether (3×20 ml) and the combined organic solutions were washed with saturated NaCl solution (1×20 ml) and dried (MgSO4). After filtration and evaporation, the residue was recrystallized from 96% ethanol to give 8.7 g (82%).

1. temperaturewas refluxed 48 h
2. customAfter evaporating off the solvent
3. dissolutionthe residue was dissolved in water (25 ml)
4. extractionThe aqueous layer was extracted with ether (3×20 ml)
5. washthe combined organic solutions were washed with saturated NaCl solution (1×20 ml)
6. dry with materialdried (MgSO4)
7. filtrationAfter filtration and evaporation
8. customthe residue was recrystallized from 96% ethanol
9. customto give 8.7 g (82%)