Neopentyl glycol diazo dinitrate(PDADN) was synthesized by one-pot process which consisted of two steps,i.e.nucleophilic substituion of 1,3-dibromo-2,2-dihydroxylmethylpropane(DBDMP) with sodium azide(SA),and nitration of the substituted intermediate (1,3-diazido-2,2-dihydroxylmethylpropane) with nitric acid(NA),but carried out in one pot without separating the intermediate. The factors affecting the yield and purity of PDADN,such as ratio of DBDMP/SA/NA,nitration temperature (T) and time (t) were investigated. The optimized process conditions were: DBDMP/SA/NA (molar ratio)=1.0/2.1/8.0,T=(15~19) ℃,and t=18 min. The yield and purity of the resulting PDADN could be up to 84% and 98% repectively,and the product′s structure was identified with IR,NMR and elemental analysis. To compare with the traditional preparation of PDADN,the one-pot process simplifies the procedures,improves PDADN′s yield and purity,mildens the reaction conditions,and is easy to be industrialized.