Carbonyl diazide (1), OC(N-3)(2), is prepared by reaction of triphosgene and tetra-n-butylammonium azide in a solution of diethyl ether or dimethyl ether. The advantage of this synthetic method, relative to other procedures, is that the use of triphosgene, OC(OCCl3)(2), mitigates the need to use highly poisonous reagents such as phosgene, OCCl2, or chlorofluorocarbonyl, OC(Cl)F. The identity and purity of OC(N-3)(2) are established by gas-phase IR spectroscopy, which reveals the presence of both syn-syn and anti-syn conformers. Computed anharmonic vibrational frequencies and infrared intensities of carbonyl diazide (1) display excellent agreement with experiment, and reveal the presence of strong Fermi resonances.