Furoxan derivatives[1-2],which have both high enthalpy of formation,high density and high oxygen balance,lead to an obvious increase in specific impulse of propellant compared to a composition of the same type containing RDX.Especially,3,4-dinitrofuroxan is a powerful energetic compound first reported in 1993[3].In addition,it would serve as an intermediate in the synthesis of other furoxan derivatives.Godovikova et al[3-4] reported the synthetic method from glyoxime via two steps of nitration and oxidation (Route A).Furthermore,3,4-dinitrofuroxan was aslo obtained by treating dinitromethane potassium salt with concentrated H2SO4 or oleum (Route B) [5].But details of two methods were incomplete.In this paper,two approaches of the synthesis of 3,4-dinitrofuroxan were carried out on the basis of literature (scheme 1),the post-processing method for dinitroglyoxime was improved.The structure of ultimate product was well confirmed by 13C NMR,14N NMR,15N NMR,IR,MS and elemental analysis,and its 15N NMR and MS spectra were obtained firstly.