1-氨基-3-十二烷基-1，2，3-三唑硝酸盐的合成研究

摘要

Amino-3-dodecyl-1,2,3-triazolium nitrate was synthesized through 4 steps including addition-elimina-tion,cyclization,alkylation and double replacement reaction by using glyoxal,hydrazine and bromododecane.The products were characterized by NMR,FT-IR and MS.The reaction conditions of addition-elimination,cyclization and alkylation were explored and optimized.The optimal conditions for each step of the reactions are as follows:In addition-elimination reaction,n(hydrazine hydrate)n(glyoxal)n(methanol)=319,70℃for 5 h with a yield of 90.3%;In cycliza-tion reaction,m(MnO2)m(glyoxal bishydrazone)=21,20℃ for 3 h with a yield of 88.2%;In alkylation reaction, n(1-amino-1,2,3-triazole)n(bromododecane)=11.5,80℃ for 40 h with a yield of 64.5%.The fourth step is a simple metathesis reaction with a high yield,in which the reaction time is 3.5h and the yield is 80.4%.The total yield of target product is 41.3%.%以乙二醛、水合肼及溴代十二烷为原料，经加成-消除、环化、烷基化、复分解4步反应得到1-氨基-3-十二烷基-1，2，3-三唑硝酸盐。通过核磁、红外、质谱等分析手段对目标产物进行了结构表征。探索并优化了加成-消除、环化和烷基化反应条件。各步反应的最佳条件为：加成-消除反应中，n（水合肼）n（乙二醛）n（甲醇）＝319，70℃反应5 h，收率为90．3％；环化反应中，m（二氧化锰）m（乙二腙）＝21，20℃反应3h，收率为88．2％；烷基化反应中，n（1-氨基-1，2，3-三唑）n（溴代十二烷）＝11．5，80℃反应40h，收率为64．5％；复分解反应易进行且得率高，反应3．5h，产率为80．4％，目标产物总收率为41．3％。