Synthesis and characterization of multidentate ligands having azo group have been subject of several researches [1-4]. We have been involved in synthesis and characterization of potentially heptadentate Schiff base ligands and corresponding metal complexes having azo group[5,6]. In this work we report the synthesis and characterization of two newpentadentate Schiff-base ligands, namely bis({[5-4-clorophenenylazo)salicylidene]amino}ethyl)amineand bis({[5-4- ethylphenenylazo)salicylidene]amino}ethyl)amine (see Fig. 1). The above ligands were synthesized by the condensation reaction ofdiethylenetriamine(1 mmol )and 5-(4-X-phenyl)-azosalicylaldehyde (X=C2H5,Cl) (2mmol) and werecharacterized using infrared,UV Visible, 1HNMRspectroscopy. Both ligands show the high extension coefficient in different solutions. The reaction of above ligands with Ni(II), Cu(II), Cd(II) and Mn(II) was also investigated. The effect of various solvents with different polaritieson the UV-Vis spectra of the all resulting compounds was also studied.