Research on The Synthesis Process of 2,4,6-Triamino-5-nitropyrimidine-1,3-dioxide
2,4,6-Triamino-5-nitropyrimidine-1,3-dioxide(ICM-102)is a new type of high-energy en-ergetic molecule with low sensitivity.The research on the synthesis of ICM-102 is beneficial for its en-gineering applications.The synthesis of 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide monohydrate(3,ICM-102·H2O)via compound 2,4,6-triamino-5-nitropyrimidine(2)was studied starting from 2,4,6-triaminopyrimidine(1).Compounds 2 and 3 were characterized by FT-IR,1H NMR,13 C NMR and HPLC.The effects of nitration systems,dosages of nitric acid and temperatures on the yields of compound 2,as well as the effects of oxidation systems,dosages of TFA and H2O2 on the yields of product 3 were studied.The optimum process conditions were obtained.Whenn(1)∶n(68％HNO3)=1.00∶3.80,temperature range is 20～50 ℃,and reaction time is 25 min,the yield of compound 2 is up to 98.8％.When n(2)∶n(30％H2O2)=1.00∶4.19,and reaction time is 8 h,the yield of 3 at room temperature is up to 71.1％.Through process study,fuming nitric acid was replaced by 68％HNO3,and the consumption of 68％HNO3 and TFA was significantly reduced.HPLC determined the purity of compound 3 as 98.1％.
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