反应详情

温度

25 °C

A solution of 3-(2,6-difluoro-3-methoxyphenyl)-4H-[1,2,4]oxadiazol-5-one (0.09 g, 0.39 mmol) in DCM (3 ml) was cooled to −78° C. followed by addition of BBr3 (0.10 ml, 1.18 mmol). The reaction mixture was stirred at 25° C. for 2 h. After the completion of the reaction mixture (TLC monitoring), solution of NaHCO3 (20 ml) was added at 0° C. and extracted with ethyl acetate (3×50 ml). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated. The crude residue was purified by column chromatography on silica (60-120 M) using ethyl acetate/hexane (50:50) as the eluent to provide the title compound as white solid (0.08 g, 95%).

1. extractionextracted with ethyl acetate (3×50 ml)
2. washThe combined organics was washed with water, brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude residue was purified by column chromatography on silica (60-120 M)