反应详情

To a solution of methyl 4-(amino(3-chloropyrazin-2-yl)methyl)benzoate (54 g, 195 mmol) in THF (500 mL) was added 2-cyanoacetic acid (16.6 g, 195 mmol) and TEA (39.4 g, 390 mmol). The mixture was added HATU (74.1 g, 195 mmol) at 0-5° C., and stirred at room temperature for 1 h. The reaction mixture was extracted with EA and water, the organic layer was dried and concentrated. The residue was purified by column chromatography on silica gel eluted with PE:EA=2:1 to give methyl 4-((3-chloropyrazin-2-yl)(2-cyanoacetamido)methyl)benzoate (67 g, yield 100%).

1. extractionThe reaction mixture was extracted with EA and water
2. customthe organic layer was dried
3. concentrationconcentrated
4. customThe residue was purified by column chromatography on silica gel
5. washeluted with PE