反应详情

To a solution of Cul (4.3 mg, 23 μmol) in triethylamine (5 ml) were added (2-ethynyl-6-methyl-pyridin-3-yl)amine (60 mg, 0.45 mmol), (PPh3)2PdCl2 (16 mg, 23 μmol), and 1,3-difluoro-5-iodobenzene (109 mg, 0.45 mmol). The reaction mixture was stirred at room temperature for 20 h. The solvent was evaporated to afford a brown oil which was taken up in DCM and the solution was washed with water. The aqueous phase was extracted twice with DCM. The organic phases were dried over Na2SO4, filtered and concentrated. The crude residue was purified by flash chromatography (hexane/ethyl acetate 7:3) to yield 64 mg (0.26 mmol, 58%) of (2-(3,5-difluoro-phenylethynyl)-6-methyl-pyridin-3-yl)amine as a yellow solid.

1. customThe solvent was evaporated
2. customto afford a brown oil which
3. washthe solution was washed with water
4. extractionThe aqueous phase was extracted twice with DCM
5. dry with materialThe organic phases were dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude residue was purified by flash chromatography (hexane/ethyl acetate 7:3)