反应详情

To a solution of N-{3-[(2-chloro-4-pyrimidinyl)acetyl]-2-fluorophenyl}-2,6-difluorobenzenesulfonamide (2.0 g, 4.53 mmol) in 40 mL DMA, 1.0 eq. NBS (0.806 g, 4.53 mmol) was added and the solution was allowed to stir 15 min at rt. 2,2-dimethylpropanethioamide (0.531 g, 4.53 mmol) was then added at rt. The reaction was heated to 60° C. for 2 hours. The reaction was not complete by LC-MS. The reaction mixture was then heated to 80° C. for an additional hour. The reaction mixture was diluted with water and extracted×2 with EtOAc. The combined EtOAc washings were washed with water×3 to remove DMA, dried over MgSO4, filtered and concentrated onto silica gel. The crude material was chromatographed in 10-80% EtOAc in Hexanes to give the desired product, 1.6 g (64%). MS (ESI): 539.1 [M+H]+.

1. temperatureThe reaction was heated to 60° C. for 2 hours
2. temperatureThe reaction mixture was then heated to 80° C. for an additional hour
3. extractionextracted×2 with EtOAc
4. washThe combined EtOAc washings were washed with water×3
5. customto remove DMA
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated onto silica gel
9. customThe crude material was chromatographed in 10-80% EtOAc in Hexanes