反应详情

To a suspension of 2-bromo-1-(2-fluorophenyl)ethanone (3.0 g) and potassium carbonate (2.0 g) in ethanol (30 mL) was added dropwise thiophenol (1.4 mL) at 0° C. The mixture was stirred at room temperature for 8 hr, insoluble materials were filtered off, and the filtrate was concentrated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=15:1) to give the title compound as a pale-yellow solid (yield 2.2 g, yield 64%).

1. filtrationinsoluble materials were filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionWater was added to the residue
4. extractionthe mixture was extracted with ethyl acetate
5. washThe extract was washed with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=15:1)