A synthesis of some new thiosemicarbazide like 1-(3-bromo-4-hydroxy-5- methoxybenzylidene)-4-(4-bromophenyl)thiosemicarbazide by condensation of 3-bromo-4- hydroxy-5-methoxybenzaldehyde with 4-(4-bromophenyl)thiosemicarbazide is carried out. And their metal complexes were synthesized by condensation of 1-(3-bromo-4-hydroxy-5- methoxybenzylidene)-4-(4-bromophenyl)thiosemicarbazide and different transition metal chloride salt of Cu(II), Co(II), Ni(II). Their characterization are done by different analytical techniques, such as elemental analysis, 1H NMR, FT-IR, GC-MS and ESI mass spectroscopy