4-Acetyldiphenyl ether and 4,4'-diacetyldiphenyl ether were synthesized from diphenyl ether and acetyl chloride in the presence of AlCl3 used as catalyst. Subsequently, their keto oxime and glyoxime derivatives were prepared. The metal complexes of the glyoximes such as Cu(II), Ni(II) and Co(II) were also prepared. The structures of these ligands and their complexes were identified by FT-IR, H-1 NMR and C-13 NMR spectral data, elemental analysis and magnetic measurements.