含能材料2025，Vol.33Issue(4)：317-323,7.DOI:10.11943/CJEM2025025
1-甲基-3,4,5-三硝基吡唑(MTNP)的简易合成
A Simple Synthesis Method of 1-Methyl-3,4,5-trinitropyrazole(MTNP)
摘要
Abstract
In order to solve the problems of high temperature and high pressure in the synthesis of 1-methyl-3,4,5-trinitropyr-azole(MTNP),a new method of simple synthesis of MTNP was developed,that is,4-chlorpyrazole(1)was used as raw materi-al,and MTNP was synthesized by nitration,N-methylation,benzylamine amination and oxidation.The effects of material ra-tios,temperatures,solvents,debenzylation reagents,and oxidation conditions on the yields of 4-benzylamino-1-methyl-3,5-di-nitropyrazole(4),4-amino-1-methyl-3,5-dinitropyrazole(5),and MTNP were investigated.Fourier transform infrared spectros-copy(FT-IR),nuclear magnetic resonance(NMR)and high performance liquid chromatography(HPLC)were used to charac-terize the structures of the intermediates and target compounds.The results showed that when the intermediate 4 was synthe-sized,the molar ratio of n(benzylamine):n(4-chloro-1-methyl-3,5-dinitropyrazole,3)=6∶1,the reaction temperature was 35℃,and petroleum ether/water was the solvent,the yield was 89.6%.In the synthesis of intermediate 5,concentrated sulfuric acid(98%)was used as debenzyl reagent,and the yield was 95.2%.The yield of MTNP was 60.5%by using intermediate 4 as substrate and"one-pot method"of debenzylation/oxidation.By optimizing the reaction conditions,the total yield of MTNP syn-thesized from raw material 1 by one-pot method was 41.5%.关键词
1-甲基-3,4,5-三硝基吡唑(MTNP)/一锅法合成/苄胺化/氧化反应Key words
1-methyl-3,4,5-trinitropyrazole(MTNP)/one-pot synthesis/benzylamination/oxidation reaction分类
武器工业引用本文复制引用
张莉,邹佳,陈政国,余思佳,李浩然,石海川,黄明,杨海君..1-甲基-3,4,5-三硝基吡唑(MTNP)的简易合成[J].含能材料,2025,33(4):317-323,7.基金项目
国家自然科学基金(22075260) （22075260）
四川省自然科学基金面上项目(2022NSFSC0288) （2022NSFSC0288）
