Three new 4-methoxybenzoylthiourea derivatives namely N-phenyl-N'-4-methoxybenzoylthiourea (A), N-(2-methoxy-phenyl)-N'-4-methoxybenzoylthiourea (B) and N-(2-nitrophenyl)-N'-4-methoxybenzoylthiourea (C) has successfully synthesized and characterized by elemental analysis, Fourier Transform Infrared (FTIR), proton ( 1 H) and carbon ( 13 C) Nuclear Magnetic Resonance (NMR) spectroscopy. Result obtained for IR showed the presence of important bands of the compounds such as ν(N-H), ν(C=O), ν(C-N) and ν(C=S) which were observed at 3200 cm -1 , 1670 cm -1 , 1200 cm -1 and 700 cm -1 , respectively. The 1 H chemical shifts for CONH and CSNH had been observed around 9 ppm and 12 ppm, respectively. For the 13 C resonance, the signal of C=O and C=S had been observed at 180 ppm and 200 ppm, respectively. The efficiency of the synthesized compounds was investigated as corrosion inhibitor of mild steel in 1.0 M H 2 SO 4 by using linear polarization resistance (LPR) technique.