Tetraacetylethylenediamine (TAED) was prepared by acetylation of diacetylethylenediamine (DAED) with acetic anhydride in a 5 L reactor coupled with a packed distillation column, 2.5 cm in inside diameter and 1 m in length. The reaction temperature was set at 135 C and the reflux ratio at 6. The molar ratio of acetic anhydride to DAED was varied from 3 to 5. A TAED yield as high as 80% was obtained, higher by 15% than in the absence of distillation. The temporal variation of the TAED yield was calculated using the kinetic parameters in the literature. Calculated and experimental values showed good agreement.