反应详情

温度

80 °C

A mixture of the piperidine from preparation 26 (220 mg, 1.91 mmol), tert-butyl 3-iodo-1-azetidinecarboxylate (600 mg, 2.0 mmol) (EP 992493) and potassium carbonate (276 mg, 2.0 mmol) in 1-methyl-2-pyrrolidinone (10 ml) was stirred at 80° C. for 48 hours. The mixture was partitioned between water and ethyl acetate, and the layers separated. The organic phase was washed with water, then brine, dried (Na2SO4), and evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel using an elution gradient of dichloromethane:methanol:0.88 ammonia (100:0:0 to 90:10:0.5) to afford the title compound, 162 mg.

1. customThe mixture was partitioned between water and ethyl acetate
2. customthe layers separated
3. washThe organic phase was washed with water
4. dry with materialbrine, dried (Na2SO4)
5. customevaporated under reduced pressure
6. customThe crude product was purified by column chromatography on silica gel using an elution gradient of dichloromethane