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4-氨基-3,5-二硝基吡唑(LLM-116)缩合物的合成与表征
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Synthesis and Characterization of 4-Amino-3,5-dinitropyrazole(LLM-116) Condensation Products
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    摘要:

    以2,4,6-三硝基氯苯、三氯三聚氰与4-氨基-3,5-二硝基吡唑(LLM-116)为原料,设计、合成了1-苦基-4-氨基-3,5-二硝基吡唑(Ⅰ)和2,4,6-三(4-氨基-3,5-二硝基吡唑-1-基)-1,3,5-均三嗪(Ⅱ)两种未见文献报道的LLM-116缩合产物,其熔点分别为: 234~236 ℃、296.5 ℃(dec.),并采用红外光谱、核磁共振光谱、元素分析等进行了结构表征。探讨了缩合反应机理,合成1-苦基-4-氨基-3,5-二硝基吡唑适宜的反应介质为N-甲基吡咯烷酮,较佳反应温度为70 ℃,时间16 h。

    Abstract:

    Taking 2,4,6-trinitrochorobenzene,2,4,6-trichoro-1,3,5-triazine and 4-amino-3,5-dinitropyrazole(LLM-116) as primary substances,1-(2,4,6-trinitrobenzene-1-yl)-4-amino-3,5-dinitro-pyrazole(Ⅰ) and 2,4,6-tri(4-amino-3,5-dinitropyrazole-1-yl)-1,3,5-triazine(Ⅱ) which have not been reported in the literature were synthesized by condensation reaction. Their structures were confirmed by IR,NMR and element analysis,and their melting point are 234-236 ℃,296.5 ℃(dec.),respectively. The condensation reaction mechanism was discussed,and the optimal reaction conditions synthesizing 2,4,6-trichoro-1,3,5-triazine are as follows: reaction medium is N-methyl-2-pyrrolidone(NMP),temperature is 70 ℃ and time is 16 h.

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王伯周,汪营磊,张志忠,等.4-氨基-3,5-二硝基吡唑(LLM-116)缩合物的合成与表征[J].含能材料, 2009, 17(3):293-295. DOI:10.3969/j. issn.1006-9941.2009.03.010.
WANG Bo-zhou, WANG Ying-lei, ZHANG Zhi-zhong, et al. Synthesis and Characterization of 4-Amino-3,5-dinitropyrazole(LLM-116) Condensation Products[J]. Chinese Journal of Energetic Materials, 2009, 17(3):293-295. DOI:10.3969/j. issn.1006-9941.2009.03.010.

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  • 收稿日期: 2008-07-23
  • 最后修改日期: 2008-10-09
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  • 在线发布日期: 2011-11-04
  • 出版日期: 2009-06-25