反应详情

To 3 ml of tetrahydrofuran/0.5 ml of distilled water, 7-bromo-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine (80.0 mg, 0.37 mmol), 2-trifluoromethyl-phenyl boronic acid (78 mg, 0.41 mmol), potassium carbonate (103 mg, 0.74 mmol) and tetrakis triphenylphosphine palladium (21 mg, 0.02 mmol) were added and then stirred at 800 for 2 hours. After completion of the reaction, the mixture was extracted with ethyl acetate, and the combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography on amine silica eluting with a solvent of dichloromethane:methanol=50:1. The fractions containing the product were collected and evaporated to obtain 7-(2-trifluoromethyl-phenyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine as white solid (67 mg, 64%).

1. customAfter completion of the reaction
2. extractionthe mixture was extracted with ethyl acetate
3. dry with materialthe combined organic layer was dried over anhydrous sodium sulfate (Na2SO4)
4. filtrationfiltered
5. customevaporated under reduced pressure
6. customThe residue was purified by column chromatography on amine silica eluting with a solvent of dichloromethane
7. additionThe fractions containing the product
8. customwere collected
9. customevaporated