反应详情

A stirred solution of 4-[4-((S)-1-{[2-(4-amino-2-chloro-5-methoxy-phenyl)-ethyl]-tert-butoxycarbonyl-amino}ethyl)-phenyl]piperazine-1-carboxylic acid tert-butyl ester (0.28 g, 0.475 mmol) and phenyl 5-cyanopyrazin-2-ylcarbamate (0.091 g, 0.38 mmol) in DMF (18 mL) was heated to 100° C. for 1 hour. The mixture was allowed to cool to room temperature, diluted with water (50 mL) and extracted with EtOAc (2×40 mL). The combined organic extracts were washed with water (3×40 mL), brine (40 mL), dried (Na2SO4) and concentrated under reduced pressure. The residue was purified with column chromatography on neutral silica gel using 25% EtOAc in hexane to give the title compound (0.16 g, 46%).

1. extractionextracted with EtOAc (2×40 mL)
2. washThe combined organic extracts were washed with water (3×40 mL), brine (40 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified with column chromatography on neutral silica gel using 25% EtOAc in hexane