反应详情

To a solution of 3,4-difluorophenylacetic acid (ALDRICH CHEMICAL) (10 g) and 2-bromo-1-(4-(methylsulfonyl)phenyl)ethanone (Lactone 11, Step 1) (17.3 g) in acetonitrile (200 mL) at r.t. was added slowly Et3N (20.2 mL). After 1 hr at r.t., the mixture was cooled in an ice bath and treated with 17.4 mL of DBU. After 2 hr 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 in a sintered glass funnel, eluted with 75% EtOAc/hexane, giving after evaporation of the solvent and a swish in EtOAc, 10 g of the title compound.

1. temperaturethe mixture was cooled in an ice bath
2. waitAfter 2 hr at 0° C.
3. extractionthe product was extracted with EtOAc
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue was applied on top of a silica gel plug in a sintered glass funnel
7. washeluted with 75% EtOAc/hexane
8. customgiving
9. customafter evaporation of the solvent