The recovery of caproic acid from the aqueous stream is of practical relevance due to its market value and the stringent environmental standards. The profound success of reactive extraction has been noted in the recovery of carboxylic acids from dilute solutions. In the present paper, the equilibrium of caproic acid with tri-n-butyl phosphate (TBP), an organophosphorous compound, in xylene and methyl isobutyl ketone (MIBK) has been studied. Equilibrium parameters such as the distribution coefficients, loading ratio, and degree of extraction have been presented. The data obtained are useful in understanding the equilibrium characteristics and efficient design of the recovery process of caproic acid by reactive extraction.