反应详情

温度

80 °C

The product of step 2 (252 mg, 0.890 mmol, 1.00 equiv), 1H-indazol-5-amine (142 mg, 1.07 mmol, 1.20 equiv), EDC (229 mg, 1.07 mmol, 1.20 equiv), and DMAP (10 mg, catalytic) were suspended in 4.0 mL DMF. Et3N (0.298 mL, 2.14 mmol, 1.00 equiv) was added and the solution was heated to 80° C. for 2 hours. The reaction mixture was cooled to room temperature and diluted with EtOAc and 1N HCl. The phases were separated, and the organic phase was washed twice with 1N HCl, once with satd. NaHCO3, and once with satd. NaCl. The organic phase was dried over Na2SO4, filtered, and concentrated en vacuo. The residue was purified by flash chromatography (100% EtOAc) to provide 0.100 g (28%) of the title compound as a white solid. MS (ES+) m/e 399 [M+H]+

1. temperatureThe reaction mixture was cooled to room temperature
2. customThe phases were separated
3. washthe organic phase was washed twice with 1N HCl, once with satd
4. dry with materialThe organic phase was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated en vacuo
7. customThe residue was purified by flash chromatography (100% EtOAc)