反应详情

To a suspension of N-azetidin-3-yl-acetamide (17) (1.99 mmol) and 2-[4-(2-bromo-ethoxy)-3,5-dimethyl-phenyl]-5,7-dimethoxy-3H-quinazolin-4-one (18) (1.00 mmol) in anhydrous DMF (10 mL) was added triethylamine (3 mL). The reaction mixture was stirred at room temperature for 3 days under nitrogen. The solvent was evaporated under reduced pressure, water (50 mL) was added, and the precipitated solid was filtered off. The aqueous layer was extracted with ethyl acetate (2×100 mL). The organic phase was dried over anhydrous Na2SO4 and concentrated. The crude compound was purified by the Simpliflash system (0-5% 7 N ammonia in methanol and CH2Cl2 as eluent) to give the title compound 19 as a white solid.

1. customThe solvent was evaporated under reduced pressure, water (50 mL)
2. additionwas added
3. filtrationthe precipitated solid was filtered off
4. extractionThe aqueous layer was extracted with ethyl acetate (2×100 mL)
5. dry with materialThe organic phase was dried over anhydrous Na2SO4
6. concentrationconcentrated
7. customThe crude compound was purified by the Simpliflash system (0-5% 7 N ammonia in methanol and CH2Cl2 as eluent)