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1-甲基-3-氨基-5-硝基-1,2,4-三唑的合成新工艺
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西安近代化学研究所,西安近代化学研究所,西安近代化学研究所

作者简介:

周群(1967-),女,高级工程师,主要从事含能材料合成研究。

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New Synthetic Process of 1-Methyl-3-amino-5-nitro-1,2,4-triazole
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Xi’an Modern Chemistry Research Institute,Xi’an Modern Chemistry Research Institute,Xi’an Modern Chemistry Research Institute

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    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。

    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.

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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. DOI:10.3969/j. issn.1006-9941.2012.01.007.
ZHOU Qun, WANG Bo-zhou, 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. DOI:10.3969/j. issn.1006-9941.2012.01.007.

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历史
  • 收稿日期: 2011-01-07
  • 最后修改日期: 2011-03-05
  • 录用日期: 2011-03-23
  • 在线发布日期: 2012-02-23
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