反应详情

Dissolve the product of Step 4 (3.93 g, 11.7 mmoles) in 50 ml of dry EtOAc. Add 4-hydroxy-4-phenyl-1-piperidine (2.55 g, 14.4 mmoles), followed by dry Et3N (13.3 ml.). Heat under N2 at 60°-65° C. for 28 h. Cool to room temperature, filter the solid and wash with EtOAc. Apply the filtrate to a silica gel column and elute the column with 1.5% CH3OH(NH3)/ETOAc. Yield: 2.34 g; Cl-MS: m/e=432 (M+H+, 35C1 +37Cl isotope).

1. temperatureHeat under N2 at 60°-65° C. for 28 h
2. filtrationfilter the solid
3. washwash with EtOAc
4. washApply the filtrate to a silica gel column and elute the column with 1.5% CH3OH(NH3)/ETOAc