Experimental data for the production of diacetone alcohol (DAA) with catalytic distillation (CD) are presented and discussed. CD has several advantages over conventional fixed-bed reactors since acetone conversions which exceed the equilibrium limit can be obtained, and no cooling of the acetone feed is required. The presence of a consecutive reaction whereby DAA is dehydrated to mesityl oxide (MV) permits an examination or the effect of catalytic distillation on product selectivity. It was found that the DAA production rate in the catalytic distillation column is controlled by external mass transfer. The catalyst activity and product selectivity of the reaction toward DAA can be improved by controlling the liquid distribution in the column.