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In this study, N-(2,4,6-tribromophenyl)maleimide (TBPMI) was synthesized using three different catalysts, including stannous chloride, anhydrous acetic acid, and phosphoric acid, respectively. Comparative analysis was carried out on the synthesis conditions and the yields of TBPMI synthesized using different catalysts. Infrared spectroscopy and nuclear magnetic resonance spectroscopy were employed to characterize TBPMI. Results showed that the use of phosphoric acid as the catalyst required harsh reaction conditions and also the catalytic efficiency was poor. On the other hand, under similar conditions, the catalytic efficiency of anhydrous acetic acid was higher than that of stannous chloride, along with the reduction in problems associated with erosion and pollution.