反应详情

4-(2-Bromo-4-nitrophenoxy)piperidine (10.96 mmol, 3.3 g), 2-(4-(bromomethyl)-phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (10.96 mmol, 3.69 g) and potassium carbonate (32.9 mmol, 4.54 g) were combined in acetonitrile (40 mL) and the mixture stirred at room temperature overnight. The mixture was concentrated under reduced pressure and the resulting residue dissolved in dichloromethane (150 mL). The organic phase was washed with water (2×50 mL) then brine (50 mL). The organic phase was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluting with dichloromethane to 10% methanol/dichloromethane) to afford the title compound (5.25 g). MS (ESI) m/z 558.8 [M+H]+

1. concentrationThe mixture was concentrated under reduced pressure
2. dissolutionthe resulting residue dissolved in dichloromethane (150 mL)
3. washThe organic phase was washed with water (2×50 mL)
4. dry with materialThe organic phase was dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography (eluting with dichloromethane to 10% methanol/dichloromethane)