- 4,5-dicyano-1,2,3-triazole—a promising precursor for a new family of energetic compounds and its nitrogen-rich derivatives: Synthesis and crystal structures
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The nitrogen-rich compounds and intermediates with structure of monocyclic, bicyclic, and fused rings based on 1,2,3-triazole were synthesized and prepared by using a promising precursor named 4,5-dicyano-1,2,3-triazole, which was obtained by the cyclization reaction of diaminomale-onitrile. Their structure and configurational integrity were assessed by Fourier transform-infrared spectroscopy (FT-IR), mass spectrometry (MS), and elemental analysis (EA). Additionally, fourteen compounds were further confirmed by X-ray single crystal diffraction. Meanwhile, the physical properties of four selected compounds (3·H2 O, 6·H2 O, 10·H2 O, and 16) including thermal stability, detonation parameters, and sensitivity were also estimated. All these compounds could be consid-ered to construct more abundant 1,2,3-triazole-based neutral energetic molecules, salts, and complex compounds, which need to continue study in the future in the field of energetic materials.
- Cao, Wenli,Qin, Jian,Sinditskii, Valery P.,Zhang, Jianguo
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- Preparation method of nitrogen-containing aromatic dicarboxylic acid
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The invention discloses a preparation method of nitrogen-containing aromatic dicarboxylic acid. The method includes: taking quinoline, isoquinoline, benzimidazole or benzotriazole and a derivative thereof as the raw materials, adopting oxone as the oxidant, employing a metal salt as the catalyst and using inorganic acid as the medium, adding a phase transfer reagent, and carrying out reaction to obtain nitrogen-containing aromatic dicarboxylic acid. The reagents used by the method are high in stability, convenient for transportation and storage, the operation is simple, the conditions are easily controllable, and the price is low, at the same time, the catalytic effect is good, the yield is high, and waste liquid treatment is easy, therefore the method is convenient for industrial large-scale production.
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Paragraph 0145-0148
(2020/03/02)
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- Green environmentally friendly 1-H-1,2,3-triazole preparation method
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The invention discloses a green environmentally friendly 1-H-1,2,3-triazole preparation method. The method uses benzotriazole and hydrogen peroxide as raw materials, 1-H-1,2,3-triazole-4,5-dicarboxylic acid is obtained under the action of a catalyst through oxidative ring opening and then acid adjusting, toluene is subjected to reflux decarboxylation, 1-H-1,2,3-triazole is obtained, the method isgreen, clean and low-cost, the product total yield can reach 80%, the purity is more than 99%, and the method is suitable for industrial production.
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Paragraph 0031; 0032; 0034; 0035; 0037; 0038; 0040; 0041
(2019/04/29)
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- 1,2,3-triazole synthesizing method
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The invention discloses a 1.1,2,3-triazole synthesizing method which comprises the following steps: performing oxidizing reaction on benzotriazole through a potassium permanganate saturated solution to obtain a solution containing 1,2,3-triazole-4,5-dicarboxylic acid; adding a hydrogen peroxide solution into the solution containing 1,2,3-triazole-4,5-dicarboxylic acid, performing suction filtration when purple of the solution fades, concentrating filtrate to obtain a concentrated solution, adding concentrated hydrochloric acid into the concentrated solution, standing, dissolving white solid out, filtering and drying to obtain 1,2,3-triazole-4,5-dicarboxylic acid; adding a solvent and cyclohexanedione into 1,2,3-triazole-4,5-dicarboxylic acid to perform decarboxylic reaction to obtain 1,2,3-triazole. According to the 1,2,3-triazole synthesizing method disclosed by the invention, the raw materials are simple and easy to obtain, reaction conditions are mild, operation is simple, aftertreatment is convenient, a requirement for equipment is not high, reaction is complete, byproducts are few, no solid waste is generated, and purifying means of filtering, centrifuging, recrystallizing andthe like are avoided.
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Paragraph 0032-0034; 0036-0038; 0040-0042; 0044-0046
(2019/02/03)
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- Synthesis method for 1H-1,2,3-triazole
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The invention provides a synthesis method for 1H-1,2,3-triazole. The synthesis method comprises the following steps of (a) oxidizing with potassium permanganate in an acid condition by using benzotriazole as a starting material and tetrabutylammonium bromide as a catalyst, so as to obtain 1H-1,2,3-triazole-4,5-dicarboxylic acid; and (b) under catalysis of N,N-diisopropylethylamine, removing the carboxyl group of the 1H-1,2,3-triazole-4,5-dicarboxylic acid, so as to obtain 1H-1,2,3-triazole. In the synthesis method, the oxidization ring-opening reaction of benzotriazole is carried out with potassium permanganate as an oxidant in the acid condition. The potassium permanganate has high oxidization in the acid condition, and the benzotriazole reacts fully, so that the yield of the 1H-1,2,3-triazole-4,5-dicarboxylic acid is improved. In step (b), water is used as a solvent and can be evaporated in post-treatment to be recycled. The synthesis method uses simple materials easy to obtain, the reaction conditions are mild, the operations are simple, the yield is high, the prepared 1H-1,2,3-triazole product has high quality, and the reaction cost is low. The synthesis method is applicable to industrial production.
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Paragraph 0032; 0038; 0039; 0043; 0044; 0048; 0049
(2017/08/31)
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- Preparation method of high-purity 1H-1,2,3-triazole
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The invention relates to a preparation method of high-purity 1H-1,2,3-triazole. The preparation method comprises steps as follows: step (1), benzotriazole is taken as a raw material, potassium permanganate is taken as an oxidizing agent, water is taken as a solvent, and high-purity 1H-1,2,3-triazole-4,5-dicarboxylic acid is obtained through an oxidation ring-opening reaction, purification and drying under the alkaline condition; step (2), 1H-1,2,3-triazole-4,5-dicarboxylic acid obtained in the step (1) has a decarboxylic reaction in an N,N-dimethylformamide solvent under the catalytic action of a catalyst, a target product, namely, high-purity 1H-1,2,3-triazole is obtained through purification, and the catalyst is quinolone, pyridine or a mixture of quinolone and pyridine. In the step (2), quinolone or pyridine is taken as a catalyst to replace conventional copper powder or oxide of copper, the reaction selectivity is good, the yield is high, the product purity is high, and the stability is better.
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Paragraph 0030; 0031; 0032
(2016/10/07)
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