反应详情

In a 10 ml flask, 1-[4-(2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-7-yl)-phenyl]-ethanone (59 mg, 0.23 mmol) and 3,5-dibromo-4-methoxy-benzoyl chloride (287 mg, 0.87 mmol) were dissolved in dichloromethane. Triethylamine (0.32 ml, 2.3 mmol) was added thereto and then stirred at room temperature for 12 hours. After completion of the reaction by adding water dropwise, the mixture was extracted with dichloromethane, 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. The fractions containing the product were collected and evaporated to obtain 1-{4-[1-(3,5-dibromo-4-methoxy-benzoyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-7-yl]-phenyl}-ethanone as white solid (119 mg, 94%).

1. customAfter completion of the reaction
2. extractionthe mixture was extracted with dichloromethane
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