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[1]刘安昌,刘芳,谭珍友,等.4氨基1,2,4三氮唑的合成[J].武汉工程大学学报,2008,(04):28-30.
 LIU An chang,LIU Fang,TAN Zhen you,et al.Study on the Synthesis of 4amino1,2,4triazole[J].Journal of Wuhan Institute of Technology,2008,(04):28-30.
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4氨基1,2,4三氮唑的合成(/HTML)
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2008年04期
页码:
28-30
栏目:
化学与化学工程
出版日期:
2008-04-30

文章信息/Info

Title:
Study on the Synthesis of 4amino1,2,4triazole
文章编号:
16742869(2008)04002803
作者:
刘安昌刘芳谭珍友肖庆张良
武汉工程大学湖北省新型反应器与绿色化学工艺重点实验室,湖北 武汉 430074
Author(s):
LIU AnchangLIU FangTAN ZhenyouXIAO Qing ZHANG Liang
Hubei Key Lab of Novel Reactor and Green Chemical Technology,Wuhan Institute of Technology, Wuhan 430074,China
关键词:
甲酸水合NN二甲酰4氨基124三氮唑
Keywords:
formic acidhydrazine hydrateNNdiformylhydrazine4amino124triazole
分类号:
TQ031.2
DOI:
-
文献标志码:
A
摘要:
以甲酸和水合肼为原料,采用缩合-环合两步法反应合成了4-氨基1,2,4三氮唑.优化影响缩合反应和环合反应的反应条件.结果表明缩合反应的最优条件为:n(甲酸):n(水合肼)=2.2∶1.0、缩合温度120 ℃、缩合时间2 h,在此条件下中间产物N,N二甲酰肼的收率为92.3%;环合反应的最优条件为:n(N,N二甲酰肼)∶n(水合肼)=1.0∶1.1、环合温度160 ℃,环合时间4 h,在此条件下4氨基1,2,4三氮唑收率为95.6%,两步反应总收率85.5%.
Abstract:
4amino1,2,4triazole was synthesized from formic acid and hydrazine hydrate by condensation and cyclocondensation. Optimize the influence of the twostep reaction conditions . Under Optimal condensation conditions: n(formic acid):n (hydrazine hydrate) = 2.2∶1.0, condensation temperature 120 ℃, condensation time 6 h, yield of intermediate N,NDiformylhydrazine is 92.3%; Under the optimal conditions of following cyclocondensation∶n(N, Nformylhydrazine)∶n(hydrazine hydrate)=1.0∶1.1, cyclocondensation temperature 160 ℃, cyclocondensation time 4 h,yield of 4amino1, 2, 4triazole is 98.6%.Overall yield of 4amino1, 2, 4triazole from above two step reactions is 91%.

参考文献/References:

[1]Quinlin W T, Cates D M.Catalytic cyclocondensation process for the synthesis of 4amino4H1,2,4triazole from hydrazine hydrate and ethyl formate:US,2005165241[P].20040127.
[2]Dionisia S, Marta P T, Alarcon S H, et al. Tautomerism in the Solid State and in Solution of a Series of 6Aminofulvene1aldimines[J]. Journal of Organic Chemistry, 2002, 67(5):14621471.
[3]Bourdauducq, P. Process for the preparation of 4amino1,2,4triazoles:EP,841328[P].19980513.
[4]Werner W,Depreux P. Reactions with formic acid. Part 2. Formohydrazides by azeotropic distillation[J]. Journal of Chemical Research, 1980,(11):372.
[5]Grigoryan G V, Agbalyan S G. New methods for preparation of 4amino1,2,4triazole[J]. Armyanskii Khimicheskii Zhurnal,1991, 44(7/8): 479481.
[6]Kost A N, Gents F. Reactions of hydrazine derivatives. XIX. Condensations of 4amino1,2,4triazole with esters[J]. Zhurnal Obshchei Khimii, 1958, 28:27732779.
[7]Quinlin, W T, Cates D M.Catalytic cyclocondensation process for the synthesis of 4amino4H1,2,4triazole from hydrazine hydrate and ethyl formate:US,2005165241[P].20050728.
[8]Drake G,Hawkins T,Brand A. Energetic lowmelting salts of simple heterocycles[J]. Propellants Explosives Pyrotechnics,2003,28(4):174180.
[9]Nasu R, Shimura T. Preparation of 4amino1,2,4triazole:JP,04308582[P]. 19921030.

相似文献/References:

[1]王威,熊祥祖*,雷琴,等.黄磷生产线上联产甲酸和磷酸钠盐[J].武汉工程大学学报,2008,(03):14.
 WANG Wei,XIONG Xiang zu,LEI Qin,et al.Preparation of formic acid and cogeneration of mixture of phosphate[J].Journal of Wuhan Institute of Technology,2008,(04):14.

备注/Memo

备注/Memo:
收稿日期:20080306
作者简介:刘安昌(1964),男,江西吉安人,教授,博士.
研究方向:精细有机合成及药物中间体合成.
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