反应详情

To a solution of 8-bromo-2-methyl-2H-1,4-benzoxazin-3(4H)-one (1.20 g, 4.96 mmol) in 1,2-dimethoxyethane (50 ml) were added 2,4-dimethylphenylboronic acid (818 mg, 5.45 mmol), tetrakis(triphenylphosphine)palladium(0) (286 mg, 0.245 mmol) and 2M sodium carbonate solution (4.96 ml, 9.92 mmol). The mixture was refluxed for 16 h and diluted with water. The aqueous solution was extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate and concentrated under vacuum. The residue was purified by column chromatography eluting with 20% ethyl acetate/n-hexane to afford 1.20 g (91%) of the title compound.

1. temperatureThe mixture was refluxed for 16 h
2. extractionThe aqueous solution was extracted with ethyl acetate
3. washThe extract was washed with brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under vacuum
6. customThe residue was purified by column chromatography
7. washeluting with 20% ethyl acetate/n-hexane