反应详情

3-Azido-6-fluoro-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one (2.25 g, 10.22 mmol), cesium carbonate (4.65 g, 14.30 mmol), and 2,2,2-trifluoroethyl trifluoromethanesulfonate (2.67 mL, 18.39 mmol) in DMF (34.1 mL) heated to 40° C. for 1 hour. The reaction mixture was diluted with water before EtOAc was added to extract the product. The organic phase was separated and washed with water (2×) and brine (1×) before being dried with Na2SO4 and evaporated to yield the crude product. This material was chromatographed on silica gel (0-80% EtOAc in hexanes) to yield 2.534 g of 3-azido-6-fluoro-1-(2,2,2-trifluoroethyl)-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one as an orange/brown solid.

1. additionwas added
2. extractionto extract the product
3. customThe organic phase was separated
4. washwashed with water (2×) and brine (1×)
5. dry with materialbefore being dried with Na2SO4
6. customevaporated
7. customto yield the crude product
8. customThis material was chromatographed on silica gel (0-80% EtOAc in hexanes)