A number of N - substituted -N’-[4-(-methyl/phenyl- 2,4- dihydro - 3H - 1,2,4- triazole - 3- thione -5- yl) phenyl] thiourea derivatives were obtained by the reactions of 5- (4- aminophenyl)-4- methyl- 2,4 - dihydro- 3H-1,2,4- triazole -3- thione with methyl,allyl, phenyl and p- bromophenyl isothiocyanates; and also by the reactions of 5- (4- aminophenyl) -4- phenyl - 2,4 - dihydro-3H-1,2,4 - triazole - 3 - thione w,th methyl, ethyl, allyl, cyclohegzyl, phenyl and p - chlorophenylisothiocyanates. The structures and purity of synthesised compounds were confirmed using UV, IR and MASS spectroscopic techniques. Compounds (V c,d, i, j) exhibited no molecular ion peaks in the mass spectra were also confirmed with elemental analysis. Keywords :