In this paper, the Taguchi method was used for the optimization of the reaction parameters for the synthesis of 2,6,8,12-tetraacetyl-4,10-dibenzyl-2 ,4 ,6 ,8 , 10 ,12-hexaazatetr acycl o [5,5,0,03,11, 05,9]dodecane in the presence of Pd(OH)2/Al2O3 catalyst in a batch suspension reactor. In order to achieve optimal conditions for this reaction, the experimental studies were conducted under varying reaction parameters, such as temperature, pressure, catalyst to substrate weight ratio, reaction time, and co-catalyst amount. The setting of the reaction parameters was determined in Qualitek-4 (Nutek (R)) software using the Taguchi experimental design method. Identification of the significant factors and their attributed levels in the Taguchi method were statistically performed via the analysis of variance (ANOVA) technique.