AbstractAzidodinitromethyl compounds represent a new highly energetic class of propellant ingredients. Preparation of these materials was accomplished by means of electroxidative coupling of azide ions to dinitromethyl carbanions. Thus, anodic coupling of sodium azide with ethyl 4,4‐dinitrobutyrate produced ethyl 4‐azido‐4,4‐dinitrobutyrate. Similarly, 4‐azido‐4,4‐dinitrobutyl acetate was prepared from 4,4‐dinitrobutyl acetate and converted by way of the corresponding alcohol to the nitrate ester, 4‐azido‐4,4‐dinitrobutyl nitrate.