Abstract Mechanistic and spectroscopic investigations of reactive C 3 H 2 hydrocarbons necessitated the preparation of diazopropyne isotopomers bearing mono-13 C substitution at each of the three unique positions. The diazo compounds and their tosylhydrazone precursors were prepared from the mono-13 C isotopomers of propynal (in the form of either the aldehyde or the diethyl acetal). The introduction of 13 C-labeling at either alkyne ...