反应详情

To a solution of 3,5-dichlorobenzyl 4-(2-((tert-butoxycarbonyl)(methyl)amino)ethyl)piperidine-1-carboxylate (step 2) (2.73 g, 6.13 mmol) in DCM (20 mL) was added trifluoroacetic acid (19 ml, 247 mmol). The reaction mixture was stirred at room temperature for 1 hour. The mixture was concentrated under pressure and the residue was suspended in sat. sodium bicarbonate solution (100 ml). The resultant mixture was extracted with EtOAc (2×100 ml). The organic portion was dried using MgSO4, filtered and concentrated under reduced pressure. The oil was applied to a 40 g silica cartridge in DCM and eluted with 0-20% MeOH/DCM containing 1% aqueous ammonia to afford the title compound;

1. concentrationThe mixture was concentrated under pressure
2. extractionThe resultant mixture was extracted with EtOAc (2×100 ml)
3. customThe organic portion was dried
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. washeluted with 0-20% MeOH/DCM containing 1% aqueous ammonia