反应详情

In a 5 ml flask, 7-trifluoromethyl-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine (27 mg, 0.23 mmol) and 3,5-dibromo-4-methoxy-benzoyl chloride (65 mg, 0.20 mmol) were dissolved in dichloromethane (0.6 ml), and then triethylamine (0.55 ml, 0.33 mmol) was added thereto dropwise at 0□. After stirring for 4 hours at room temperature, water was added and the mixture was extracted with ethyl acetate. 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 silica eluting with a solvent of methanol:dichloromethane=1:100. The fractions containing the product were collected and evaporated to obtain white solid (64 mg, 98%).

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