Abstract: A series of xanthenedione derivatives have been efficiently synthesized from condensation reaction between aromatic aldehydes and 1,3-cyclohexanedione or 5,5-dimethyl-1,3-cyclohexane dione which co-catalyzed by hexamolybdate and benzyl triethyl ammonium chloride (BTEAC). In addition, the reaction solvent, composite catalyst and composite catalyst dosage have been studied. The catalytic system can be easily seperated and reused up to four times without loss of catalytic activities. All synthetic compounds have been identified and characterized by means of melting point, IR, 1H NMR, 13C NMR, MS and X-ray diffraction analysis, and the possible reaction mechanism has been proposed.