摘要
以1,3-二硝基吡唑为原料,经热重排、氨气中和得到3,5-二硝基吡唑铵盐,然后酸化得到3,5-二硝基吡唑。以三甲基肼碘化物(TMHI)作为异常亲核取代氢(VNS)反应试剂,与3,5-二硝基吡唑在叔丁醇钾为催化剂,利用VNS反应合成4-氨基-3,5-二硝基吡唑(LLM-116)。采用红外分析、核磁共振、元素分析等仪器鉴定了其结构,讨论了VNS反应机理及影响因素。通过实验,得出最佳VNS反应试剂为TMHI,反应时间为4h,反应温度为25℃,收率达到60%。
3, 5-Dinitropyrazole ammonium salt was synthesized by rearranging 1, 3-dinitropyrazole as initial material and bubbling ammonia, and acidified to 3,5 dinitropyrazole. 1,1,1 Trimethyhydrazinium iodide（TMHI） as a VNS agent was reacted with 3,5-dinitropyrazole in the presence of t-Buok as catalyst to get 4-amino-3,5- dinitropyrazole （LLM 116） through the VNS reaction. Their structures were confirmed by IR, NMR, MS and elemental analyses. The VNS reaction mechanism and factors of influencing the reaction were discussed. The results show that under optimal condition of TMHI as VNS reation reagent and the reaction at 25 ℃ for 4h, the yield of LLM-116 was 60%.
出处
《火炸药学报》
EI
CAS
CSCD
2007年第6期20-23,共4页
Chinese Journal of Explosives & Propellants
