反应详情

4-(Pyridine-3-yloxy)ethynylbenzene (50 mg, 0.256 mmol), cupric sulfate (12.26 mg, 0.077 mmol), sodium ascorbate (20.30 mg, 0.102 mmol), and 3-azido-6-fluoro-1-(2,2,2-trifluoroethyl)-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one (93 mg, 0.307 mmol) in 2.5 mL of a 1:1:1 solution of DMF:EtOH:H2O was stirred for 25 mins. The mixture was diluted with water and 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 afford an oil. This material was chromatographed on silica (0-80% EtOAc in hexanes to yield 75.7 mg as a 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 afford an oil
8. customThis material was chromatographed on silica (0-80% EtOAc in hexanes
9. customto yield 75.7 mg as a solid