反应详情

温度

130 °C

A mixture of N-(2-bromo-4-fluorophenyl)-2-cyanoacetamide (5.00 g, 19.4 mmol), (3E)-4-methoxybut-3-en-2-one (2.33 g, 23.3 mmol), 1,4-diazabicyclo[2.2.2]octane (2.18 g, 19.4 mmol) and 2-(2-methoxyethoxy)ethanol (50 mL) was stirred at 130° C. for 5 hr. After cooling to room temperature, the mixture was diluted with ethyl acetate, washed with 1N hydrochloric acid, water (×2) and saturated brine, dried over anhydrous magnesium sulfate, and filtered through a silica gel pad. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (100 g, ethyl acetate/hexane=2/98→50/50), washed with ethyl acetate-hexane and collected by filtration to give the title compound (1.78 g, 29%) as a pale-brown powder.

1. temperatureAfter cooling to room temperature
2. washwashed with 1N hydrochloric acid, water (×2) and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered through a silica gel pad
5. customThe solvent was evaporated under reduced pressure
6. customthe obtained residue was purified by silica gel column chromatography (100 g, ethyl acetate/hexane=2/98→50/50)
7. washwashed with ethyl acetate-hexane
8. filtrationcollected by filtration