2-methyl-2-nitro-1-azidopropane was synthesized from 2-methyl-2-nitropropanol via a two-step procedure. The structure of the targeted product was confirmed by Fourier transform infrared spectroscopy(FTIR),nuclear magnetic resonance(NMR).According to the study of experimental conditions,the optimum conditions for the synthesis of 2-methyl-2-nitropropyl methanesulfonate were that using triethylamine as acid binding agent and trimethylamine hydrochloride as catalyst,the ratio of reactants is(n）2-methyl-2-nitropropanol: (n) MsCl: (n) Et3N: (n) Me3N.HCl= 1: 1.2: 1: 0.05.And then, the optimum conditions for the synthesis of 2-methyl-2-nitroazepine were determined as follows:(n) 2-methyl-2-nitro-propyl methanesulfonate: (n) NaN3=1:1.5,(DMSO: water )volume=10:1 ,and the reaction was carried out at 120℃ for 24 h.The yield can be increased from 30% to 93.7%. After two steps of optimization, we can obtain the target compound that was high yield as well as more suitable for industrial production.