Aiming at the problems of high reaction temperature, easy to produce toxic and harmful gases, many side effects, low yield, and difficult product recovery of organic chemistry comprehensive experiments in the textbook, the experiment of “Synthesis of 1-Benzyl-2-Phenylbenzimidazole” was designed. This experiment had strong comprehensiveness, including the basic operation of organic chemical experiment and column chromatography, thin layer chromatography (TLC), melting point determination and nuclear magnetic determination, and ChemDraw, MetReNova and other software were used to analyze and process data. This experiment is suitable for senior undergraduates, which effectively avoids some problems existing in the current organic chemistry comprehensive experiment oxidation and reduction experimental project, so that the comprehensive experimental ability of undergraduates majoring in chemical industry can be exercised.