CHINESE JOURNAL OF ENERGETIC MATERIALS
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新法合成5-氨基四唑
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胡奂(1985-),女,硕士研究生,从事四唑类高氮含能化合物及其配合物的合成研究。e-mail: pita3204@sina.com.cn

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国家自然科学基金资助(10976014)


New Synthetic Route of 5-Aminotetrazole
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    摘要:

    以氨基胍硝酸盐为原料,重氮化后,调节反应溶液至弱碱性,加热分子内环化得到5-氨基四唑,并采用红外光谱、核磁共振光谱、质谱等方法,进行了结构表征。探讨了5-氨基四唑合成反应机理,考察了环化反应溶液酸碱性、反应温度及反应时间等关键因素对反应的影响,获得适宜反应条件为: 重氮化反应pH=2~3、温度为20~30 ℃、时间为0.5 h,环化反应溶液pH=8~9,温度为85~90 ℃,反应3.5 h,5-氨基四唑的收率达77.2%。

    Abstract:

    5-Aminotetrazole was synthesized via a novel route by diazotization and intramolecular cyclization conditioning the reaction system at basic,and aminoguanidine nitrateas as starting material. The resulting 5-aminotetrazol was characterized by IR,13C NMR,and Ms etc. The mechanism of the reaction was proposed. The key factors affecting the yield,such as acidity or basicity of reaction system,reaction temperature and time, were also investigated. The optimized procedures are as follows: for diazo-reaction: pH=2~3,T=20~30 ℃ and t=0.5 h; for intramolecular cyclization: pH=8~9,T=85~90 ℃ and t=3.5 h. The yield of 5-aminotetrazole could be up to 77.2%.

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胡奂,杨红伟,程广斌,等.新法合成5-氨基四唑[J].含能材料, 2011, 19(3):269-271. DOI:10.3969/j. issn.1006-9941.2011.03.006.
HU Huan, YANG Hong-wei, CHENG Guang-bin, et al. New Synthetic Route of 5-Aminotetrazole[J]. Chinese Journal of Energetic Materials, 2011, 19(3):269-271. DOI:10.3969/j. issn.1006-9941.2011.03.006.

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历史
  • 收稿日期: 2010-08-03
  • 最后修改日期: 2011-01-06
  • 录用日期: 2010-11-04
  • 在线发布日期: 2012-02-22
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