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1-甲基-3-氨基-5-硝基-1,2,4-三唑的合成新工艺
引用本文:周群,王伯周,贾思媛.1-甲基-3-氨基-5-硝基-1,2,4-三唑的合成新工艺[J].含能材料,2012,20(1):26-29.
作者姓名:周群  王伯周  贾思媛
作者单位:西安近代化学研究所,陕西西安,710065
摘    要:以甲基肼为原料,与盐酸反应得到盐酸甲基肼,再与二氰二胺在50℃进行缩合环化反应,调节溶液pH值,经重氮化反应合成含能化合物1-甲基-3-氨基-5-硝基-1,2,4-三唑(DNMT),总收率62.3%,纯度99.4%,并用红外光谱、核磁共振、质谱、元素分析等方法表征了其结构。探讨了缩合环化反应工艺条件,确定适宜的反应条件为:溶剂为乙醇,n(C2H3N4)∶n(NH2NHCH3.2HCl)=1∶1.1,pH=8~9,成盐组分是盐酸,重结晶溶剂为丙酮。

关 键 词:有机化学  含能材料  二氰二胺  1-甲基-3-氨基-5-硝基-1  2  4-三唑(DNMT)  合成
收稿时间:1/7/2011 12:00:00 AM
修稿时间:3/5/2011 12:00:00 AM

New Synthetic Process of 1-Methyl-3-amino-5-nitro-1,2,4-triazole
ZHOU Qun,WANG Bo-zhou and JIA Si-yuan.New Synthetic Process of 1-Methyl-3-amino-5-nitro-1,2,4-triazole[J].Chinese Journal of Energetic Materials,2012,20(1):26-29.
Authors:ZHOU Qun  WANG Bo-zhou and JIA Si-yuan
Affiliation:(Xi′an Modern Chemistry Research Institute,Xi′an 710065,China)
Abstract:A new energetic compound,1-methyl-3-amino-5-nitro-1,2,4-triazole (DNMT),was synthesized using a new synthetic process from hydrazine dihydrochloride and methyl hydrazine as starting material via condensation,cyclization and diazo-reaction. The yield of DNMT was 62.3% and its purity was more than 99.4%. The structure of DNMT was characterized by IR,MS,NMR and elemental analysis. The condensation synthetical process were discussed in detail. The optimum reaction condition was as follow: alcohol as reaction solvent, n(C2H3N4):n(NH2NHCH3·2HCl)=1:1.1,pH=8-9,hydrochloric acid as acidifying agent,acetone as recryctallization solvent.
Keywords:organic chemistry  energetic materials  hydrazine dihydrochloride  1-methyl-3-amino-5-nitro-1  2  4-triazole (DNMT)  synthesis
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