Abstract: The method of utilizing .alpha.,.beta.-unsaturated amino acids, acyl, and N-acyl derivatives as linking agents in the solid phase synthesis of peptides with the corresponding production of carboxyl terminal amides. Preferred unsaturated amino acids are dehydroalanine and dehydrobutyrine which are constituents in naturally occurring amides such as nisin and subtilin. The synthesis follows conventional lines of R. B. Merrifield et al including blocking of the amino nitrogen, with the exception that the release agent contains an amount of water equimolar to the reactant .alpha.,.beta.-unsaturated amino acid.