One-pot nitrene/carbene transfer and post-functionalization of N-heterocyclic scaffolds. Both the nitrene and carbene transfer steps can be telescoped into a single pot (Scheme 7A) using an Ntosyloxycarbamate 5 as the nitrene precursor. Treatment of 5 with Rh2(esp)2 and K2CO3 to achieve the aziridination was followed by treatment with 2c to give a mixture of 4cc and 3cc in 60% yield over the two steps.