反应详情

To a tetrahydrofuran solution (1 mL) of 4-bromo-5-(4-fluorobenzyloxy)-2-{4-[(2-tetrahydropyranyl)oxy]phenyl}-2H-pyridazin-3-one (136 mg, 0.29 mmol), 2.66 N n-butyl lithium hexane-solution (0.13 mL, 0.35 mmol) was added at −78° C. and stirred for 30 minutes. Methanol was added to the reaction liquid, warmed up to room temperature and ethyl acetate was added. Thus obtained organic layer was washed with 5% aqueous citric acid solution and saturated brine, and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the resulting residue was purified on silica gel column chromatography (C-300; ethyl acetate:hexane=1:1) to provide the title compound (74.2 mg, 65.3%).

1. washThus obtained organic layer was washed with 5% aqueous citric acid solution and saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. concentrationConcentrating the solvent under reduced pressure
4. customthe resulting residue was purified on silica gel column chromatography (C-300; ethyl acetate:hexane=1:1)