[1]蒋燕飞,叶志文.1-氨基-3-十二烷基-1,2,3-三唑硝酸盐的合成研究[J].爆破器材,2013,42(05):6-12.[doi:10.3969/j.issn.1001-8352.2013.05.002]
　JIANG Yanfei,YE Zhiwen.Synthesis of 1-Amino-3-Dodecyl-1,2,3- Triazolium Nitrate[J].EXPLOSIVE MATERIALS,2013,42(05):6-12.[doi:10.3969/j.issn.1001-8352.2013.05.002]
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1-氨基-3-十二烷基-1,2,3-三唑硝酸盐的合成研究()
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《爆破器材》[ISSN:1001-8352/CN:32-1163/TJ]

卷:
42
期数:
2013年05
页码:
6-12
栏目:
基础理论
出版日期:
2013-10-20

文章信息/Info

Title:
Synthesis of 1-Amino-3-Dodecyl-1,2,3- Triazolium Nitrate
文章编号:
4637
作者:
蒋燕飞; 叶志文
南京理工大学化工学院（江苏南京，210094）
Author(s):
JIANG Yanfei; YE Zhiwen
School of Chemical Engineering, Nanjing University of Science and Technology( Jiangsu Nanjing, 210094)
关键词:
含能表面活性剂; 乙二醛双腙; 1-氨基-3-十二烷基-1; 2; 3-三唑硝酸盐; 合成
Keywords:
energetic surfactant; glyoxal bishydrazone ;  1-amino-3-dodecyl-1; 2; 3-triazolium nitrate;  synthesis
分类号:
TQ56 O621.2
DOI:
10.3969/j.issn.1001-8352.2013.05.002
文献标志码:
A
摘要:
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%。
Abstract:
Amino-3-dodecyl-1, 2, 3-triazolium nitrate was synthesized through 4 steps including addition-elimination, 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 cyclization 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%.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期：2013-05-17
作者简介：蒋燕飞（1989~），女，硕士，主要从事表面活性剂的研究。
通信作者：叶志文（1968~），男，教授，主要从事表面活性剂及含能材料方面的研究。
更新日期/Last Update: 2013-11-06