Abstract:N-Methyl-N-(2-nitroxyethyl)nitramine (Me-NENA),N-ethyl-N-(2-nitroxyethyl)nitramine (Et-NENA) and N-butyl-N-(2-nitroxyethyl)nitramine (Bu-NENA) were prepared by the reactions of methyl ethanolamine,ethyl ethanolamine,butyl ethanolamine and nitric acid,acetic anhydride respectively. The structure of the target products were identified by 1H NMR,IR and elemental analysis. The parameters affecting the yield and purity of Et-NENA,such as temperature,reaction time,nitric acid and acetic anhydride were discussed. The optimum conditions were given: n(ethyl ethanolamine):n(nitric acid):n(acetic anhydride)=1:2.6:2.4,the reaction temperature of the first stage 5-10 ℃,the second reaction temperature 40-45 ℃,reaction time 15 min,yield of Et-NENA was over 84.70% and the purity of the refined product was over 98.07%. The physical,chemical,safety properties and thermol decomposition of alkyl-NENAs have been experimentally studied.