摘要
以亚氨基二乙腈为起始原料,经过亚硝基化、环合、硝化三步反应得到2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。确定了硝化2,6-二氨基吡嗪-1-氧化物(DAPO)制备LLM-105的最佳工艺条件为:反应温度25℃,反应时间5h,用发烟硝酸或硝酸钾向发烟硫酸和2,6-二氨基吡嗪-1-氧化物混合物中加料的工艺路线,总产率为35%。用1 H NMR,IR,MS对DAPO和LLM-105的结构进行了表征,推测了DAPO环化反应历程。
A new synthetic method using iminodiacetonitrile as the starting material in three steps including nitrosy- lation, cyclization and nitration was designed to prepare 2,6-diamino-3,5-dinitropyrazine-l-oxide （LLM-105）. The optimal reaction conditions for preparing LLM 105 via 2,6-diamino pyrazine-l-oxide（DAPO） were as follows： the reaction temperature 25℃, the reaction time 5h and fuming nitrate acid or potassium nitrate added to the mixture of fuming sulfuric acid and DAPO with total yield of 35%. The structures of DAPO and LLM 105 were determined by 1HNMR, IR, MS spectra. The mechanism of DAPO cyclization reaction was speculated.
出处
《火炸药学报》
EI
CAS
CSCD
北大核心
2012年第3期15-17,共3页
Chinese Journal of Explosives & Propellants
作者简介
赵晓锋（1983-），男，博士研究生，从事含能材料合成研究。
