反应详情

In a 5 ml flask, 7-trifluoromethyl-1H-pyrido[2,3-b][1,4]oxazin-2-one (60 mg, 0.28 mmol) was dissolved in tetrahydrofuran (1.0 ml), and then 1.0M Lithium aluminum hydride dissolved in tetrahydrofuran (0.33 ml, 0.33 mmol) was added thereto dropwise and stirred for 1 hour at 0□. Water and saturated solution of sodium hydrogen carbonate were 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=1:50. The fractions containing the product were collected and evaporated to obtain white solid (29 mg, 52%).

1. additionwas added
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 silica eluting with a solvent of methanol
7. additionThe fractions containing the product
8. customwere collected
9. customevaporated