反应详情

To a stirred solution of 1-(1-(4-(4-piperidinyloxy)-5-fluoro-2-methoxybenzoyl)piperidin-4-yl)-4H-3,1-benzoxazin-2(1H)-one of Example 16 (200 mg, 0.41 mmol) in DCM (5 mL) at ambient temperature was added acetic anhydride (77 mg, 0.75 mmol) and DIEA (0.17 mL, 1.0 mmol). The solution was stirred at ambient temperature for 24 h, diluted with DCM (20 mL), washed with saturated aqueous NaHCO3 (50 mL), dried (MgSO4), and filtered. The solvent was removed under reduced pressure and the residue was purified by pressurized silica gel column chromatography using a gradient elution of 2-5% MeOH-DCM. 1-(1-(4-(N-acetyl-4-piperidinyloxy)-5-fluoro-2-methoxybenzoyl)piperidin-4-yl) -4H-3,1-benzoxazin-2(1H)-one was obtained as an amorphous solid.

1. washwashed with saturated aqueous NaHCO3 (50 mL)
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. customThe solvent was removed under reduced pressure
5. customthe residue was purified by pressurized silica gel column chromatography
6. washa gradient elution of 2-5% MeOH-DCM