Catalytic activity of HRhCO(TPPTS)(3) intercalated hydrotalcite (Mg/Al molar ratio =3.5) as a multifunctional catalyst [HT(3.5)-INT] was studied for synthesis of C-8 aldehydes (2-ethylhex-2-enal and 2-ethylhexanal) from propylene in a single pot. The effect of catalyst amount, partial pressure of propylene, and aldol temperature (T-2) on the selectivity of 2-ethylhexanal and 2-ethylhex-2-enal was studied in detail to optimize the reaction parameters. The highest selectivity for C-8 aldehydes (49%) was obtained at 1200 mg of catalyst and 10 atm partial pressure of propylene. Reusability experiments revealed that the HRhCO(TPPTS)(3) intercalated hydrotalcite shows activity even after fourth cycle for hydroformylation reaction; however, selectivity of C-8 aldehydes decreased after the second cycle. Rates of the product formation were determined individually for hydroformylation of propylene, aldol condensation of n-butanal, and hydrogenation of 2-ethylhex-2-enal catalyzed by [HT(3.5)-INT] using propylene, n-butanal, and 2-ethylhex-2-enal as reactants. Reaction conditions were maintained identical to those used for the single-pot synthesis of C-8 aldehydes from propylene. The calculated rates of reaction for the single-pot synthesis of C-8 aldehydes were compared with the rates of reaction determined individually.