反应详情

To a solution of 1.0 g (2.336 mmol) of the product of Example 202 in 7.5 mL of DMF was added 0.50 g (2.804 mmol) of ethynyl biphenyl, 0.033 g (0.047 mmol) of bis triphenylphosphine palladium(II) dichloride 4.4 mg of copper(I) iodide and 7.5 mL of triethylamine. The reaction was heated to 80° for 5 h and then diluted with ether. the organics were washed with water, 5% HCl solution and sodium bicarbonate solution, dried over MgSO4, filtered and concentrated in vacuo. The residue was chromatographed on silica gel cluting with EtOAc/hexanes (1:3) to provide 0.777 g (63%) of the alkyne as a brown foam. Electrospray Mass Spec: 526.2 (M+H)+.

1. temperatureThe reaction was heated to 80° for 5 h
2. washthe organics were washed with water, 5% HCl solution and sodium bicarbonate solution
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was chromatographed on silica gel cluting with EtOAc/hexanes (1:3)