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 hours at ambient temperature, the reaction solution was concentrated. The residue was then dissolved in acetic acid (30 mL). After stirring at ambient temperature for 2 hours, the solvent was removed. The residue was partitioned between ethyl acetate and 5% aqueous NaHCO3. The organic layer was dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography (EtOAc/Hexanes) to provide 1-3 as a off-white solid (3.32 g, 81%). 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. stirringAfter stirring at ambient temperature for 2 hours
4. customthe solvent was removed
5. customThe residue was partitioned between ethyl acetate and 5% aqueous NaHCO3
6. dry with materialThe organic layer was dried over Na2SO4
7. concentrationconcentrated
8. customThe residue was purified by silica gel chromatography (EtOAc/Hexanes)