反应详情

1,2-Dimethoxyethane (8 mL) and water (2 mL) were added to the mixture of ethyl 5-(bromomethyl)isoxazole-3-carboxylate (1.00 g; 4.27 mmol), 2,5-difluorophenylboronic acid (0.773 g; 4.70 mmol), tetrakis(triphenylphosphine)palladium(0) (0.248 g; 0.640 mmol) and sodium carbonate (0.911 g; 8.55 mmol). The mixture was irradiated in a microwave oven at 130° C. for 20 minutes. After cooling, the reaction mixture was extracted with ethyl acetate and water. The organic layer was concentrated under reduced pressure and the residue was purified by flash chromatography on silica gel (eluent: 5 to 40% of ethyl acetate in heptane) to give 0.67 g (59%) of ethyl 5-(2,5-difluorobenzyl)isoxazole-3-carboxylate as a yellow oil.

1. customThe mixture was irradiated in a microwave oven at 130° C. for 20 minutes
2. temperatureAfter cooling
3. extractionthe reaction mixture was extracted with ethyl acetate and water
4. concentrationThe organic layer was concentrated under reduced pressure
5. customthe residue was purified by flash chromatography on silica gel (eluent: 5 to 40% of ethyl acetate in heptane)