反应详情

A stirred solution of tert-butyl-4-(4-(((4-amino-2-chloro-5-methoxyphenethyl)(tert-butoxycarbonyl)amino)methyl)phenyl)piperazine-1-carboxylate (0.46 g, 0.800 mmol) and phenyl 5-cyanopyrazin-2-ylcarbamate (0.153 g, 0.64 mmol) in DMF (18 mL) was heated to 100° C. for 1.5 hours. The mixture was allowed to cool to room temperature, diluted with water (40 mL) and extracted with EtOAc (2×30 mL). The combined organic extracts were washed with water (3×15 mL), brine (10 mL), dried (Na2SO4) and concentrated under reduced pressure. The residue was purified with column chromatography on neutral silica gel using 1.5% methanol in DCM to give the title compound (0.25 g, 43%).

1. extractionextracted with EtOAc (2×30 mL)
2. washThe combined organic extracts were washed with water (3×15 mL), brine (10 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified with column chromatography on neutral silica gel using 1.5% methanol in DCM