4,4'-Bis(chloroacetyl)diphenyl ether (HL) was synthesized from chloroacetyl chloride and diphenyl ether in the presence of AlCl 3 as catalyst by Friedel-Crafts reaction. Subsequently, its keto oxime (H 2 L) and glyoxime (H 4 L) derivatives were also prepared. Then, five new substituted 4,4'-oxy-bis(aminophenylglyoximes) (H 4 L 1-5 ) were synthesized from 4,4'-oxy-bis(chlorophenylglyoxime) and the corresponding amines. The Ni(II), Cu(II), and Co(II) complexes of these ligands were prepared. The structures of these ligands and their complexes were identified by FT-IR, 1 H NMR, and ICP-AES spectral data, elemental analyses, and magnetic measurements. ş ş