反应详情

According to Scheme 6 Step 1: A solution of 1-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)-2-bromoethanone (8.39 mmol, 3.00 g), KF (33.6 mmol, 1.97 g) and 18-crown-6 (4.20 mmol, 1.12 g) in acetonitrile (25 mL) was stirred under reflux for 3 hours. After the evaporation of solvent, the crude residue was dissolved in AcOEt. The organic phase was washed with water, was dried over Na2SO4, was filtered and was concentrated. The resulting crude product was purified by flash chromatography over silica gel using DCM/MeOH (100:0 to 95:5) as eluent to yield 1-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)-2-fluoroethanone (3.62 mmol, 900 mg, 78%) as a white solid.

1. temperatureunder reflux for 3 hours
2. customAfter the evaporation of solvent
3. dissolutionthe crude residue was dissolved in AcOEt
4. washThe organic phase was washed with water
5. dry with materialwas dried over Na2SO4
6. filtrationwas filtered
7. concentrationwas concentrated
8. customThe resulting crude product was purified by flash chromatography over silica gel