反应详情

1-2 (3.0 g, 12.75 mmol) was dissolved in THF (64 mL) and N-methylbenzene-1,2-diamine (2.02 g, 16.58 mmol), EDC (2.93 g, 15.30 mmol), HOAt (2.08 g, 15.30 mmol), and Hunig's base (6.7 mL, 38.3 mmol) were added. After stirring for 18 h at room temperature, the reaction solution was concentrated. The residue was then dissolved in acetic acid (30 mL), stirred at room temperature for 2 h, the solvent was concentrated under reduced pressure. The residue was partitioned between ethyl acetate and 5% aqueous NaHCO3. The organic layer was dried over Na2SO4, filtered, and concentrated. The crude residue was purified by silica gel chromatography (EtOAc/Hexanes) to provide 1-3 as an off-white solid. MS: m/z=322.4 (M+H).

1. concentrationthe reaction solution was concentrated
2. dissolutionThe residue was then dissolved in acetic acid (30 mL)
3. stirringstirred at room temperature for 2 h
4. concentrationthe solvent was concentrated under reduced pressure
5. customThe residue was partitioned between ethyl acetate and 5% aqueous NaHCO3
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude residue was purified by silica gel chromatography (EtOAc/Hexanes)