[O:1]=[C:2]1[CH:7]=[C:6]([CH:8]=[O:9])[CH:5]=[CH:4]N1.Cl[C:11]([F:16])([F:15])C([O-])=O.[Na+].[CH3:18]N(C=O)C>C(#N)C.C(OCC)(=O)C>[F:15][CH:11]([F:16])[O:1][C:2]1[CH:7]=[C:6]([CH:5]=[CH:4][CH:18]=1)[CH:8]=[O:9]To a solution of 2-oxo-1,2-dihydropyridine-4-carbaldehyde (1.72 g, 11.3 mmol) in 25 mL of acetonitrile was added sodium chlorodifluoroacetate (0.925 g, 7.51 mmol). The reaction was heated to reflux under an atmosphere of nitrogen for 15 h, and then DMF (3 mL) was added. The mixture was heated to 100° C. for 3 d, cooled to rt, and diluted with ethyl acetate. The organic solution was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo to provide 3-(difluoromethoxy)benzaldehyde.
Wird geladen…
