反应详情

The product of Example 3 Step 2 (250 mg, 0.881 mmol, 1.00 equiv), 5-amino-7-chloroindazole (148 mg, 0.881 mmol, 1.0 equiv), and EDC (203 mg, 1.06 mmol, 1.20 equiv) were suspended in 2.0 mL DMF. Et3N (0.148 mL, 1.06 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 38 mg (10%) of the title compound as an off white solid. MS (ES+) m/e 434 [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)