《2,6-二氨基-3,5-二硝基-1-氧吡嗪合成工艺的改进》.pdf.pdf

10 火炸药学报 Chinese Journal ofExplosives&Propellants 第35卷第2期 2年4月 2,6~二氨基~3,5一二硝基一1一氧吡嗪合成工艺的改进郁晓宇,陆明,聂福德(1_南京理工大学化工学院,江苏南京210094 ,四川I绵阳621900) 摘要:以2,6二氯吡嗪为原料,经过甲氧基化、硝化、氨化、氧化合成出2,6-二氨基3,5-二硝基1氧吡嗪(I。I,IVI 105)。研究了甲氧基化条件、硝化体系、氨化条件、三氟乙酸与双氧水的体积比等因素对LLM一105总产牢的影响。得到优化的合成条件是:质量分数2 5%的甲醇钠甲醇溶液,回流3h;用质量分数20%发烟硫酸和硝酸钾硝化体系硝化2,6- h;质子溶剂乙醇作为氨化溶剂,60。C下反应2 h;三氟乙酸与质量分数30% 双氧水的体积比3:2,45℃下反应6h;u。M 105的总收率达到54%。关键词:有机合成;钝感炸药,2,6-二氨基一3,5-二硝基一卜氧吡嗪;I,I。M一105;合成工艺中图分类号:TJ55;TQ2] 文献标志码:A 文章编号:1007—7812(2012)02—0010 05 Improvement ofthe Synthesis Process of2,6-Diamino-3,5-Dinitropyrazine-1一Oxide YU Xiao—yu,LU Ming,NIE Fu—de School ofChemical Engineering,Nanjing University ofScience and Technology,Nanjing 210094,China Chemical Materials,China Academy Engineering Physics,Mianyang Sichuan ) Abstract:LLM一105 was prepared by methoxytation,nitration,amination,and oxidation using 2,6-dichloropyrazine as starting effects rIlethoxylaLioII reaction condition,different nitration system,different amination system and volunRe ratiooftrifluoroacetic acid and hydrogen peroxide on the totalyield ofI。LM一105 were investiga— synthesis conditions are 25%sodium methoxide methan01 for ,6 Dimethoxy— pyrazine as intermediate fornitration,20%oleum and potasMum nitrate nitration systenl,the reaction at[ooIn perature for s