反应详情

温度

120 °C

To a solution of 2-cyano-N-(2,4-difluorophenyl)acetamide (5.5 g, 28 mmol) and (3E)-4-methoxybut-3-en-2-one (3.65 g, 36.5 mmol) in dimethyleneglycol monomethylether (50 mL) was added 1,4-diazabicyclo[2.2.2]octane (3.14 g, 28 mmol), and the mixture was stirred at 120° C. for 12 hr. The reaction mixture was diluted with 2N hydrochloric acid, tetrahydrofuran and ethyl acetate, and extracted 3 times with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered. The solvent was evaporated under reduced pressure. The obtained residue was washed with ethyl acetate to give a slightly yellow solid. The slightly yellow solid was suspended in tetrahydrofuran at 80° C., and the suspension was stirred for 30 min. The suspension was filtrated, and the obtained solid was washed with tetrahydrofuran to give the title compound (650 mg, 9.4%) as a white solid.

1. extractionextracted 3 times with ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customThe solvent was evaporated under reduced pressure
6. washThe obtained residue was washed with ethyl acetate
7. customto give a slightly yellow solid
8. stirringthe suspension was stirred for 30 min
9. filtrationThe suspension was filtrated
10. washthe obtained solid was washed with tetrahydrofuran