【作者】 周诚； 李祥志； 王伯周； 王锡杰； 霍欢；

【Author】 ZHOU Cheng;LI Xiang zhi;WANG Bo zhou;WANG Xi jie;HUO Huan;Xi’an Modern Chemistry Research Institute;

【机构】 西安近代化学研究所；

【摘要】 研究了一种高安全性合成1,1-二氨基-2,2-二硝基乙烯(FOX-7)的方法,以盐酸乙脒与乙二酸二乙酯为原料,经环化反应合成了2-甲氧基-2-甲基-4,5-咪唑烷二酮,再经硝硫混酸硝化、水解反应得到了1,1-二氨基-2,2-二硝基乙烯(FOX-7),总收率为56.7%。考察了硝化剂、反应温度、反应时间等因素对硝化反应收率的影响,确定了最佳硝化反应条件:以硝硫混酸(硝硫混酸体积比为1:2)为硝化剂,反应温度为15~20℃,反应时间为1h,收率可达到62.8%。更多还原

【Abstract】 A synthetic method for 1,1-diamino-2,2-dinitroethylene(FOX-7) with high security was studied. 2-Methoxy-2-methylimidazolidine-4,5-dione was prepared via cyclization using acetamidinium chloride and diethyl oxalate as starting materials, and FOX-7 was synthesized by the nitration with HNO3-H2SO4, hydrolysis with water, in a yield of 56.7%. The effects of nitration of mixed acid volume ratio, reaction temperature, reaction time on the yield were investigated. The optimal process conditions of nitration was detemined as HNO3-H2SO4(the volume ratio is 1:2), reaction temperature 15~20 ℃, reaction time 1h. Under these conditions, the yield of FOX-7 is 62.8%.更多还原