Symmetrically and unsymmerically substituted bis-dithiobenzil nickel complexes containing four substituted and unsubstituted methoxy groups were synthesized from a benzoin compound using phosphorous pentasulfide under the conventional thermal and microwave processing. The efficiency of microwave synthesis over the conventional thermal synthesis was illustrated by the yield of bisdithiobenzil nickel complex dyes. The samples were characterized by the means of elemental analyzer, (HNMR)-H-1, IR spectroscopy, Uv-vis spectroscopy and DSC.