A model peptide, N-carbobenzoxy-L-phenylalanyl-L-phenylalanine methyl ester, was synthersized with free and immobilized thermolysin in a microaqueous system. The model peptide was formed mostly during the initial phase of the reaction. The yields of the compound with free and immobilized thermolysin after 4hr of reaction were 77.8 and 71.2, respectively.