Method for preparing 1,3,5-trinitropyrazole by electrochemical method

A technology for nitropyrazole and dinitropyrazole, which is applied in the field of electrochemical synthesis of 1,3,5-trinitropyrazole, can solve the problems of difficult post-processing, many side reactions, and high reaction cost, and achieves The effect of good substrate universality, high yield and simple reaction process

Inactive Publication Date: 2021-12-03
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these reaction systems are very corrosive to equipment, and produce a large amount of waste acid and waste water containing organic compounds, causing serious environmental pollution and high treatment costs.
In addition, these methods have poor selectivity, long reaction time, low product yield, high reaction cost, many side reactions, and difficult post-processing, etc.

Method used

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  • Method for preparing 1,3,5-trinitropyrazole by electrochemical method
  • Method for preparing 1,3,5-trinitropyrazole by electrochemical method
  • Method for preparing 1,3,5-trinitropyrazole by electrochemical method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026]

[0027] Under stirring at room temperature, slowly add 1.5 g of 1,3-dinitropyrazole into a flask containing 12 mL of o-dichlorobenzene, raise the temperature in the sand bath to 175 ° C, and stir at constant temperature for 8 h. After the reaction is completed, the reaction solution is cooled to Cool in an ice-water bath at room temperature, filter under reduced pressure to obtain the crude product of C-nitropyrazole, add an appropriate amount of diethyl ether to the crude product, reflux and stir for 0.5h, cool down in an ice-water bath and filter, remove diethyl ether in a vacuum, and obtain relatively pure 3,5-nitropyrazole base pyrazole.

Embodiment 2

[0029] Other conditions are the same as in Example 1, and the experiments of different reaction times are checked, and the experimental results are shown in Table 1.

[0030] The influence of table 1 reaction time on productive rate

[0031]

Embodiment 3

[0033] Other conditions are the same as in Example 1, and the experiments of different reaction temperatures are checked, and the experimental results are shown in Table 2.

[0034] The influence of table 2 temperature of reaction on productive rate

[0035]

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Abstract

The invention discloses a method for preparing 1,3,5-trinitropyrazole through an electrochemical method, an N-nitropyrazole compound is prepared through electrochemistry, economical and nontoxic metal nitrate is used as a nitro source. According to the invention, a novel construction method of a trinitropyrazole energetic compound is realized through the reaction, by which a target product is obtained at a high yield under a constant current. The pyrazole ring structure has large ring tension and contains high-energy N-N bonds and C-N bonds. The nitro group is introduced on the ring, so that the density and the nitrogen content are increased, and the oxygen balance is closer to an ideal value, thereby improving the detonation performance of the compound.

Description

technical field [0001] The invention belongs to the technical field of energetic materials, and relates to a method for synthesizing 1,3,5-trinitropyrazole by an electrochemical method. Background technique [0002] Azacyclazole compounds are widely used in many fields such as medicine, pesticides, materials, etc., and are quite popular among people. Nitropyrazole compounds are one of the important compounds. Nitropyrazole compounds are aromatic and stable substances, which are characterized by oxidation resistance, heat resistance, and hydrolysis resistance, and can be widely used in medicine, pesticides, photosensitive materials, and fine chemicals. There is a π-electron system on the pyrazole structure, and the ring is easy to undergo reactions such as electrophilic substitution, nitration, iodination, and halogenation. After nitration, nitropyrazole can be obtained. The mass fraction of nitrogen in nitropyrazole derivatives is higher than that of carbon and hydrogen, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/09C25B3/20
CPCC25B3/09C25B3/20
Inventor 王鹏程邹洁冬陆明林秋汉许元刚
Owner NANJING UNIV OF SCI & TECH
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