Novel 1-(p-aniinophenyl)-3-(p-substituted -phenyl)-5-phenylforrnazan compounds (2a-f) and 1,1'-(1,1'-biphenyl]-4-4'-yl)bis(3-(p- substituted pheny1)-5-plienylformazan compounds (3a-f) were synthesized by diazo coupling reactions of the prepared hydrazOnes (1a-f) With diazoniuni salts of phenylenediattine and benzidine, respectively. Novel mono=formazans were obtained with high yields under mild reaction conditions and were crystallized from methanol. Bis-forniazans Were purified by flash column chromatograph over silica gel. The strtictures of formazans and bis-fottimzans were confirmed by elemental analysis; HR MS and their spectral behaviours were investigated using H-1 NMRs; C-13 NMR, FT-IR techniques. The absorption characteristicsof the compotinds were examined by UV-visible spectra.