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Preparation Process and Mechanism of Cutting off the C─N Research of Sodium Pentazole Salt
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1.School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China;2.The Gansu Yinguang Chemical Industry Group Co. LTD, Baiyin 730999, China

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    Abstract:

    Sodium pentazole salt was prepared by treating 2, 6-dimethyl-4-(2H-pentazol-2-yl) phenolate with m-chloroperbenzoic acid (m-CPBA) and ferrous bisglycinate [Fe(Gly)2] under low-temperature conditions, thereinto, m-CPBA and Fe(Gly)2 were oxidizer and catalyst, respectively. The synthetic conditions were optimized, as following:the molar ratio between arylpentazole, Fe(Gly)2 and m-CPBA was 1:3:4.5, the reaction time was 24 h and the reaction temperature was-45 ℃(crude yield of 28%). The effect of different oxidizing cleavage reagents on the yield of sodium pentazole salt was studied and the reason for the low yield of sodium pentazole salt was analyzed. In addition, sodium pentazole salt and the reaction by-product (2, 6-dimethylcyclohexa-2, 5-diene-1, 4-dione) were characterized by X-ray single crystal diffractometer (XRD), NMR (15NMR and 1H NMR), FT-IR, mass spectrometry and elemental analysis. Based on these results, the mechanism of oxidizing cleavage of the C─N bond in arylpentazole by m-CPBA and Fe(Gly)2 was speculated.

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邵艳丽,王乾,王鹏程,等.五唑钠的制备工艺及C─N键切断机理[J].含能材料,2018,26(11):925-930.
SHAO Yan-li, WANG Qian, WANG Peng-cheng, et al. Preparation Process and Mechanism of Cutting off the C─N Research of Sodium Pentazole Salt[J]. Chinese Journal of Energetic Materials,2018,26(11):925-930.

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History
  • Received:May 08,2018
  • Revised:September 29,2018
  • Adopted:August 28,2018
  • Online: September 13,2018
  • Published: November 25,2018