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Employing <jats:italic>N<\/jats:italic>,<jats:italic>N<\/jats:italic>\u2032\u2010disuccinimidyl carbonate to activate benzophenone hydrazone, we have developed a more efficient approach for the synthesis of aza\u2010glycinyl dipeptides. Alkylation of the semicarbazone of the resulting protected aza\u2010glycinyl dipeptides using tetraethylammonium hydroxide and propargyl bromide provided an efficient entry into the aza\u2010propargylglycinyl peptide building blocks, which have served previously in various reactions including Sonogashira cross\u2010couplings, dipolar cycloadditions and intramolecular <jats:italic>exo\u2010dig<\/jats:italic> cycloadditions to furnish a variety of azapeptide building blocks. 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