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For effective drug design and development, an integrated process utilizing all available information from structural, thermodynamic, and biological studies plays a very important role. To understand the energy basis of molecular interactions utilizing various thermodynamic methods, volumetric and acoustic studies are vital early in the development process of any drug toward an optimal energy interaction profile while retaining a good pharmacological assay. In this article, we are reporting the data of densities (ρ) and speeds of sound (u) of an antiarrhythmic agent, namely, procainamide hydrochloride in an aqueous binary and aqueous solution of amino acids, i.e., l-alanine and l-valine at T = (298.15, 308.15 and 318.15) K. Different thermodynamic parameters such as the apparent molar volume (V ϕ) of the solute, the isentropic compressibility (κs) of the solution, and the apparent molar isentropic compressibility (κϕ) of procainamide hydrochloride in water and aqueous solutions of l-alanine and l-valine have been computed using the density and speed of sound data at different temperatures. The limiting apparent molar volume (V ϕ 0) of solute and the limiting apparent molar compressibility (κϕ 0) of solute in binary and ternary aqueous solutions have been obtained by extrapolating the plots. The results have been interpreted in light of the competing solute–solute and solute–solvent interactions.