1,2-aceanthrylenedione was synthesized through the acylation reaction of anthracene and oxalyl chloride catalyzed by anhydrous AlCl3. The effects of various reaction conditions on the yield and selectivity of 1, 2-aceanthrylenedione were studied by GC analysis. The results show that the optimum synthesis conditions of the acylation reaction are as follows : the molar ratio of oxalyl chloride to anthracene being 1:2, the molar ratio of anhydrous AlCl3 to anthracene being 4:1, the reaction time being 5 h, the reaction temperature being 303k and the solvent of the reaction system being CS2. Under those conditions, the yield and selectivity of 1, 2-aceanthrylenedione is 83.8 % and 92.3% respectively. Pure 1, 2-aceanthrylenedione was prepared by extraction and recrystallation. The structure of 1, 2-aceanthrylenedione was identified by measure of melting point, GC/MS, FTIR and 1HNMR analyses.