2,6-二氨基-3,5-二硝基吡嗪-1-氧化物的超声快速有效合成研究
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- 英文论文题名：Fast and effective synthesis of 2,6-diamino-3,5-dinitropyrazine-1-oxide with assistance of ultrasonic technology
- 论文作者：卢欢唱 ; 廖龙渝 ; 马卿 ; 马军
- 英文论文作者：Huanchang Lu ; Longyu Liao ; Qing Ma ; Jun Ma ; Department of Chemistry Institute of Chemical Materials ; China Academy of Engineering Physics
- 年：2016
- 作者机构：中国工程物理研究院化工材料研究所;
- 论文关键词：LLM-105 ; 超声 ; 合成
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第三十四分会：公共安全化学
- 语种：中文
- 分类号：O626
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第三十四分会 ; 公共安全化学
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：170k
- 原文格式：D
- 会议级别：全国
摘要
报道了超声波作用下合成2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)的方法。即以2,6-二氨基-3,5-二硝基吡嗪(ANPZ)为原料,三氟乙酸和双氧水为氧化剂,在超声的作用下,合成LLM-105。并探讨了超声功率、超声时间等因素对LLM-105合成的影响,确定了超声合成反应的最佳超声功率、超声时间等条件。在此条件下,产物LLM-105的纯度与得率均大于95%,成功将反应时间缩短了近80%,缩短至5h。从而解决了常规氮氧化反应合成时间长(约24 h)、效率低等问题。产物LLM-105采用核磁、液相色谱、扫描电镜及光学显微镜进行了结构与纯度表征。
2,6-diamino-3,5-dinitropyrazine-1-oxide(LLM-105) was synthesized from 2,6-diamino-3,5-dinitropyrazine(ANPZ) as starting material and trifluoroacetic acid(TCA) and hydrogen peroxide as oxidizer under the ultrasonic reaction conditions. The effect of ultrasonic power and reaction time on the yield and purity of LLM-105 were investigated, and the optimal reaction conditions were obtained. The experimental results indicated that the purity and yield all exceeded 95 % under the optimized condition. Meanwhile, compared with the traditional N-oxide synthesis~([1-2])(this step may take about 24 h to accomplish), our method obviously decreased the reaction time to 5h which was nearly shorten by 80 %. The final product was further characterized by nuclear magnetism resonance(NMR), liquid-phase chromatography(LC), scanning electronic spectroscopy(SEM) and optical spectra.
2,6-diamino-3,5-dinitropyrazine-1-oxide(LLM-105) was synthesized from 2,6-diamino-3,5-dinitropyrazine(ANPZ) as starting material and trifluoroacetic acid(TCA) and hydrogen peroxide as oxidizer under the ultrasonic reaction conditions. The effect of ultrasonic power and reaction time on the yield and purity of LLM-105 were investigated, and the optimal reaction conditions were obtained. The experimental results indicated that the purity and yield all exceeded 95 % under the optimized condition. Meanwhile, compared with the traditional N-oxide synthesis~([1-2])(this step may take about 24 h to accomplish), our method obviously decreased the reaction time to 5h which was nearly shorten by 80 %. The final product was further characterized by nuclear magnetism resonance(NMR), liquid-phase chromatography(LC), scanning electronic spectroscopy(SEM) and optical spectra.
引文
[1]李海波,程碧波,李洪珍,聂福德,李金山,黄忠,刘世俊.有机化学,2007,27(1):17.
[2]邓明哲,周杰文,王伯周,叶志虎,田战怀.含能材料,2013,21(3):294.
[2]邓明哲,周杰文,王伯周,叶志虎,田战怀.含能材料,2013,21(3):294.