反应详情

Heat a mixture of 5-chloro-6-{4-[2-chloro-6-(4-fluoro-phenyl)-pyrimidin-4-yl]-piperazin-1-yl}-nicotinic acid ethyl ester (1.19 g, 0.0025 mol) and 2-methylpyrrolidine (2.5 mL, 0.025 mol) in DMA at 120° C. for 14 h. Partition the reaction mixture between EtOAc and water. Wash the organic layer with water (1×) and brine (1×), then dry (Na2SO4) and concentrate under reduced pressure. Filter the crude product through a silica gel pad (2 inches deep×3 inches in diameter) eluting with 700 mL of 30% EtOAc/hexanes. Concentrate under reduced pressure to give the title compound as an off-white foam.

1. temperatureHeat
2. customPartition the reaction mixture between EtOAc and water
3. washWash the organic layer with water (1×) and brine (1×)
4. dry with materialdry (Na2SO4)
5. concentrationconcentrate under reduced pressure
6. filtrationFilter the crude product through a silica gel pad (2 inches deep×3 inches in diameter)
7. washeluting with 700 mL of 30% EtOAc/hexanes
8. concentrationConcentrate under reduced pressure