反应详情

The product of Example 1, Step 2 (50 mg, 0.178 mmol, 1.00 equiv), 5-amino-3-methylindazole (26 mg, 0.178 mmol, 1.0 equiv), and EDC (41 mg, 0.213 mmol, 1.20 equiv) were suspended in 0.5 mL DMF. Et3N (0.030 mL, 0.213 mmol, 1.2 equiv) was added and the solution was stirred at room temperature for 18 hrs. The reaction mixture was 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 (20-100% EtOAc in Hexanes) to provide 15 mg (21%) of the title compound as an off white solid. MS (ES+) m/e 411 [M+H]+

1. customThe phases were separated
2. washthe organic phase was washed twice with 1N HCl, once with satd
3. dry with materialThe organic phase was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated en vacuo
6. customThe residue was purified by flash chromatography (20-100% EtOAc in Hexanes)