The Study On Synthesis Technology Of FOX-7and Its Derivatives

FOX-7(1,1-diamino-2,2-dinitroethylene) has the properties of high energy density andlow sensitivity, it is a typical new energetic material. The yield present is only38%, improveits yield, reduce the cost, further study to research derivatives of FOX-7with higher energyand better performance make sense for application of FOX-7and improvement of militaryequipment level. Therefore, the paper researched the synthesis of FOX-7and its derivatives.2-methyl pyrimidine-4,6-diketone was synthesized based on acetamidine hydrochlorideand malonic diethyl, sodium ethoxide and sodium methoxide as catalysts respectively. Theproduct was characterized by FT-IR spectrum. Influence of factors of temperature, time, feedratio, catalysts to yield was researched by single element experiment. The optimumconditions of synthesis was determined by orthogonal experiment. When sodium ethoxidewas selected as catalyst, the yield could be86%while molar ratio of acetamidinehydrochloride, malonic diethyl,catalyst was1:1:1.5and the reaction mixture was heated toachieve a temperature of90℃which was maintained for3h. When the catalyst was sodiummethoxide, the yield could be79%while molar ratio of acetamidine hydrochloride, malonicdiethyl, catalyst was1:1:1.5and the reaction was maintained for3h at70℃.2-(dinitromethylene)-4,5-imidazolidine diketone was synthesized by nitrating2-methylpyrimidine-4,6-diketone, then, FOX-7was got after hydrolysis reaction.The product wascharacterized by FT-IR spectrum. Influence of factors of temperature, time, feed ratio,composition of nitro-sulfuric acid, molar ratio of2-methyl pyrimidine-4,6-diketone andnitro-sulfuric acid to yield was researched by single element experiment. The optimizedconditions: molar ratio of2-methyl pyrimidine-4,6-diketone and fuming nitric was1:4,volume of fuming nitric and concentrated sulfuric was1:2.5temperature was10℃andmaintained for3h. The yield was82%.According to mechanism of aldehyde-ammonia condensation, derivatives of FOX-7with high-nitrogen: and its synthetic routes were designed. Synthesized the title compound basedon FOX-7and glyoxal when PH was alkaline. The product was purified by thin layerchromatography, columnchromatography and recrystallization, then, components wereanalysed by LC-MS,the result showed that2,5-(dinitromethylene)-octahydro imidazo [4,5-d]imidazole existed during the products.The study has guiding significance for further study of synthesis of FOX-7and itsderivatives.