反应详情

To a solution of 3,4-difluorophenylacetic acid (ALDRICH CHIMICAL) (10 g) and 2-bromo-1-(4-(methylsulfonyl)phenyl)ethanone (Example 9, Step 1) (17.3 g) in acetonitrile (200 mL) at room temperature was added slowly triethylamine (20.2 mL). After 1 h at room temperature, the mixture was cooled in an ice bath and treated with 17.4 mL of DBU. After 2 h at 0° C., the mixture was treated with 200 mL of 1N HCl and the product was extracted with EtOAc, dried over Na2SO4 and concentrated. The residue was applied on top of a silica gel plug (sintered glass funnel) eluted with 75% EtOAc/hexane, giving after evaporation of the solvent and swish in ethyl acetate, 10 g of the title compound.

1. temperaturethe mixture was cooled in an ice bath
2. waitAfter 2 h at 0° C.
3. extractionthe product was extracted with EtOAc
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. washeluted with 75% EtOAc/hexane
7. customgiving
8. customafter evaporation of the solvent