反应详情

To an N,N-dimethylformamide (50.0 mL) solution of 4-bromobenzyl alcohol (4.54 g, 24.3 mmol) was added sodium hydride (1.00 g, 25.0 mmol, 60% in oil) under nitrogen atmosphere at 0° C., which was stirred for 30 minutes at room temperature. 2-Fluoro-5-methylpyridine (1.80 g, 16.2 mmol) was then added at 0° C., and stirred for 5 hours at room temperature. Water was added to the reaction solution at room temperature, which was then extracted with ethyl acetate. The organic layer was separated and washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:15) to obtain the title compound (2.67 g, 59.3%).

1. stirringstirred for 5 hours at room temperature
2. extractionwhich was then extracted with ethyl acetate
3. customThe organic layer was separated
4. washwashed with saturated aqueous sodium chloride
5. customthe solvent was evaporated under a reduced pressure
6. customThe residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:15)