This study examined the feasibility of reacting benzoyl chloride (PhCOCl) and sodium glycinate (H2NCH2COOH) catalyzed by 4-dimethylaminopyridine (DMAP) in an alkaline (NaOH) aqueous solution/dichloromethane two-phase medium. This catalyzed reaction of benzoyl chloride and sodium glycinate was described by a pseudo-first-order rate law. The hydrolysis of benzoyl chloride in the two-phase reaction was neglected on the specified reaction conditions. In addition, the effects of operating conditions on the conversion of benzoyl chloride and the reaction rate. According to those results, the reaction rate decreases with an increasing concentration of benzoyl chloride, which contradicts the general rate law of reaction kinetics. This peculiar phenomenon could be accounted for altering the interfacial property due to the change of the chemical property of reactants and intermediate, and the interaction between reactants and intermediate which was transferred from organic phase to aqueous phase.