反应详情

温度

80 °C

(4-Amino-3-methoxy-benzyl)-benzyl-carbamic acid tert-butyl ester (0.25 g, 0.73 mmol) and phenyl 5-cyanopyrazin-2-ylcarbamate (0.21 g 0.87 mmol) (Example 10) were dissolved in DMF (2.5 mL) and heated at 80° C. for 2 hours. The mixture was allowed to cool to room temperature then partitioned between water (15 mL) and EtOAc (25 mL). The separated aqueous layer was extracted with EtOAC (25 ml), and then the combined organic extracts were washed with water (15 mL), brine (10 mL), dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by column chromatography on neutral silica gel using 15-25% EtOAc in hexane to afford the title compound (0.24 g, 67%).

1. temperatureto cool to room temperature
2. customthen partitioned between water (15 mL) and EtOAc (25 mL)
3. extractionThe separated aqueous layer was extracted with EtOAC (25 ml)
4. washthe combined organic extracts were washed with water (15 mL), brine (10 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by column chromatography on neutral silica gel using 15-25% EtOAc in hexane