Lithium hydrazonides, prepared by reactions of hydrazones with n-BuLi/hexane in THF at− 78° C, are converted by azidotris (diethylamino) phosphonium bromide in THF at∼ 0° C efficiently, rapidly, and safely to their corresponding diazo compounds along with tris (diethylamino) phosphorimine, nitrogen, and lithium bromide.