A simple and convenient method has been developed for the synthesis of 1,3,8,10,15,17,22,24-octanitrophthalocyanine derivatives MPcON's [M=Fe(III)Cl, Zn(II), Co(II), Cu(II) and Ni(II)]. The compounds were prepared from 3,5-dinitrophthalic acid in the presence of ammonium chloride, urea and catalytic quantity of ammonium molybdate in nitrobenzene solvent; the complexes were characterized by elemental analysis, electronic and IR spectra and powder XRD. The electrochemical redox properties of the complexes were studied using glassy carbon and platinum electrodes in non-aqueous media employing tetra butyl ammonium perchlorate as supporting electrolyte.