Corrosion of a material by reaction with a corrosive environment is a common problem across many industries. Iraq is an oil country and corrosion represents a large portion of the total costs for oil producing and a natural potential hazard associated with oil production and transportation. The synthesis of novel thiosemicarbazone, namely 2-(2,4-dimethoxybenzylidene)hydrazinecarbothioamide (DMBHC), was conducted and the chemical structure was elucidated via the 1H and 13C NMR (Nuclear magnetic resonance), and FT-IR (Fourier-transform infrared) spectroscopic spectroscopic techniques in addition to carbon, hydrogen, and nitrogen analyses (CHN analyses). The inhibition properties of the investigated thiosemicarbazone were evaluated for mild steel (MS) corrosion in 1N H2SO4 using electrochemical impedance spectroscopy (EIS), weight loss method, and scanning electron microscopy (SEM). Electrochemical and weight loss techniques revealed that the tested thiosemicarbazone acted as a superior inhibitor for the acidic corrosion of MS and the efficiency increased with increasing concentrations. The EIS results revealed that thiosemicarbazone demonstrated the highest inhibition efficiency of 94.86%, at a concentration of 0.5 mM. Results from the weight loss technique suggested that the thiosemicarbazone acted as a mixed type corrosion inhibitor. The impact of temperature on the mechanism of inhibition of the new synthesized inhibitor of the surface of MS in 1N H2SO4 was investigated at various temperatures (30–60 °C) where the inhibitive efficiency diminished with increasing temperatures. The mechanism of inhibition was additionally verified with the methodological data.