CHINESE JOURNAL OF ENERGETIC MATERIALS
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甲醇溶液中五氮唑负离子的制备与表征
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作者单位:

(南京理工大学化工学院, 江苏 南京 210094)

作者简介:

徐冰韬(1990-),男,硕士研究生,主要从事含能材料的合成研究。e-mail: aslman@126.com 通信联系人: 陆明(1963-),男,教授,主要从事含能材料的设计与合成研究。e-mail: luming@mail.njust.edu.cn

通讯作者:

陆明(1963-),男,教授,主要从事含能材料的设计与合成研究。e-mail: luming@mail.njust.edu.cn

基金项目:

国家自然科学基金资助(51374131)


Synthesis and Characterization of Pentazole Anion in Methanol
Author:
Affiliation:

(School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China)

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    摘要:

    以对氨基苯磺酸为起始原料, 通过重氮化、缩合和水解反应, 合成了3, 5-二甲基-4-羟基苯胺盐酸盐, 总收率为75%。用3, 5-二甲基-4-羟基苯胺盐酸盐制备了-50 ℃下稳定的3, 5-二甲基-4-羟基苯基五唑, 收率为66.7%。以甲醇为溶剂, 亚铁盐为还原剂, 间氯过氧苯甲酸为氧化剂, 可切断3, 5-二甲基-4-羟基苯基五唑分子中的C—N键, 得到少量的五唑负离子, 并通过质谱、核磁等方法对其进行表征。同位素标记实验证明五唑环中N原子具有相同的化学环境, 说明五唑负离子极有可能具有芳香性。

    Abstract:

    3, 5-Dimethyl-4-hydroxy aniline hydrochloride was synthesized with a total yield of 75% from p-aminobenzene sulfonic acid via diazotization, condensation and hydrolysis reaction. 3, 5-Dimethyl-4-hydroxy phenyl-pentazole, which is stable at-50 ℃ was synthesized from 3, 5-dimethyl-4-aniline hydrochloride, and the yield was 66.7%. A small amount of pentazole anion was synthesized from 3, 5-dimethyl-4-hydroxy phenyl-pentazole by using methanol as solvent, ferrous salts as reductant, and m-chloro-peroxybenzoicacid as oxidant to break the C—N bond. Pentazole anion was characterized by MS and NMR. According to the isotope labeling experiments, nitrogen atoms in pentazole anion are in the same chemical environment, which means pentazole anion may possess aromaticity.

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引用本文

徐冰韬,王鹏程,王乾,等.甲醇溶液中五氮唑负离子的制备与表征[J].含能材料, 2017, 25(3):215-220. DOI:10.11943/j. issn.1006-9941.2017.03.007.
XU Bing-tao, WANG Peng-cheng, WANG Qian, et al. Synthesis and Characterization of Pentazole Anion in Methanol[J]. Chinese Journal of Energetic Materials, 2017, 25(3):215-220. DOI:10.11943/j. issn.1006-9941.2017.03.007.

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历史
  • 收稿日期: 2016-09-30
  • 最后修改日期: 2017-01-13
  • 录用日期: 2016-12-21
  • 在线发布日期: 2017-03-24
  • 出版日期: 2017-03-27