反应详情

Sodium hydride (purity: 63%, 75 mg) was added to a solution of (5-chloro-6-methoxypyridin-2-yl)(4-methyl-3,4-dihydro-2H-1,4-benzoxazin-7-yl)methanol (302 mg) in tetrahydrofuran (2 mL) under ice-cooling, and the mixture was stirred with warming to room temperature overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1) to give the title compound as a yellow solid (231 mg).

1. temperaturecooling
2. extractionfollowed by extraction with ethyl acetate
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customThe solvent was then evaporated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1)