4-(Chloroacetyl) diphenyl ether ( I) was synthesized from chloroacetyl chloride and diphenyl ether in the presence of AlCl3 as catalyst in a Friedel-Crafts reaction. Subsequently, its keto oxime (II) derivative was prepared. Then 3 new substituted 4-(alkylaminoisonitrosoacetyl) diphenyl ether ligands derived from 4-(phenoxy) phenyloxylohydroxymoyl chloride and corresponding amines were synthesized. The following aromatic and aliphatic amines were used for the ligands ethanolamine, 2-amino-4- methylphenol, and 2(aminomethyl) pyridine. Mononuclear or binuclear Co(II), Ni(II), Cu(II), and Cd(II) complexes of the ligands were synthesized. The structures of these ligands were identified by FT-IR, H-1-NMR, and C-13-NMR spectral data and elemental analysis, and the structures of the complexes were identified by FT-IR, ICP-AES, elemental analysis, and magnetic susceptibility measurements.