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Preparation method of 1-methyl-3,4-binitro pyrromonazole

A technology of dinitropyrazole and methyl, which is applied in the field of preparation of 1-methyl-3,4-dinitropyrazole, can solve the problems of harsh operating conditions, low product yield, environmental pollution, etc., and achieve The raw materials are easy, the synthesis process is simple, and the effect of improving product purity and yield

Inactive Publication Date: 2013-12-25
ZHONGBEI UNIV
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  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the technical problems of high cost, low product yield, harsh operating conditions and serious environmental pollution in the existing preparation method of 1-methyl-3,4-dinitropyrazole, and provide a 1 -The preparation method of methyl-3,4-dinitropyrazole, the safe raw material content of this method is low, the synthesis process is simple, the product yield is high, the purity is high, and it is easy to industrialize

Method used

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  • Preparation method of 1-methyl-3,4-binitro pyrromonazole
  • Preparation method of 1-methyl-3,4-binitro pyrromonazole

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Effect test

Embodiment 1

[0016] First, weigh 4.36g of raw materials 3,4-dinitropyrazole, 5.75g of anhydrous potassium carbonate, 10mL of dimethyl carbonate, 41mL of N,N-dimethylformamide, and then add N,N-dimethylformamide Add amide (DMF) into a reaction vessel equipped with a stirrer and a thermometer, place the reaction vessel at a low temperature of 0-5°C, and dry and grind the fine powder of 3,4-dinitropyrazole (DNP) slowly Add in the reaction vessel, after 3,4-dinitropyrazole (DNP) dissolves completely, anhydrous potassium carbonate (K 2 CO 3 ) and dimethyl carbonate (DMC) were added to the reaction solution in the container in sequence. After the addition was complete, stir and keep warm at 60°C for 4 hours, then pour the reaction solution into a container filled with 300mL distilled water, and stir well until the liquid turned dark red. , and after oil droplets appeared, use dichloromethane (CH 2 Cl 2 ) extraction, the organic phases were combined, the solvent was removed, and benzene was re...

Embodiment 2

[0025] First, weigh 4.36g of raw materials 3,4-dinitropyrazole, 5.75g of anhydrous potassium carbonate, 15mL of dimethyl carbonate, 45mL of N,N-dimethylformamide, and then add N,N-dimethylformamide Add amide (DMF) into a reaction vessel equipped with a stirrer and a thermometer, place the reaction vessel at a low temperature of 0-5°C, and slowly add the dried and ground 3,4-dinitropyrazole (DNP) fine powder In the reaction vessel, after 3,4-dinitropyrazole (DNP) is completely dissolved, anhydrous potassium carbonate (K 2 CO 3 ) and dimethyl carbonate (DMC) were sequentially added to the reaction liquid in the container. After the addition was complete, the reaction was stirred and kept at 80°C for 4.5 hours. Red, and after the appearance of oil droplets, dichloromethane (CH 2 Cl 2 ) extraction, the organic phases were combined, the solvent was removed, and benzene was recrystallized to obtain 4.30 g of a light yellow crystal product with a yield of 90%.

[0026] The synthe...

Embodiment 3

[0033] First, weigh 4.36g of raw materials 3,4-dinitropyrazole, 5.75g of anhydrous potassium carbonate, 20mL of dimethyl carbonate, 47mL of N,N-dimethylformamide, and then add N,N-dimethylformamide Add amide (DMF) into a reaction vessel equipped with a stirrer and a thermometer, place the reaction vessel at a low temperature of 0-5°C, and dry and grind the fine powder of 3,4-dinitropyrazole (DNP) slowly Add in the reaction vessel, after 3,4-dinitropyrazole (DNP) dissolves completely, anhydrous potassium carbonate (K 2 CO 3 ) and dimethyl carbonate (DMC) were added to the reaction solution in the container in turn. After the addition, stirred and kept at 85°C for 7 hours, then poured the reaction solution into a container filled with 300mL of distilled water, and stirred until the liquid was dark red. , and after oil droplets appeared, use dichloromethane (CH 2 Cl 2 ) extraction, the organic phases were combined, the solvent was removed, and benzene was recrystallized to obt...

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Abstract

The invention relates to a preparation method of 1-methyl-3,4-binitro pyrromonazole. The 1-methyl-3,4-binitro pyrromonazole prepared through the method disclosed by the invention is high in energy and desensitization and lower in melting point and is a normal-temperature liquid explosive. The preparation method is mainly used for solving the technical problems of high cost, low yield, and the like of the traditional preparation method of the 1-methyl-3,4-binitro pyrromonazole. The technical scheme is as follows: the preparation method comprises the following steps: weighing raw materials according to the condition that the ratio of the amount of substance of 3,4-binitro pyrromonazole:anhydrous potassium carbonate:dimethyl carbonate:N,N-dimethyl formamide is 1:1.5:(5-13):20-25); dissolving the 3,4-binitro pyrromonazole into the N,N-dimethyl formamide at the low temperature of 0-5 DEG C, and then sequentially adding the anhydrous potassium carbonate and the dimethyl carbonate; reacting at 60-110 DEG C for 4-10 hours; pouring reaction liquid into distilled water; extracting for multiple times by using dichloromethane (CH2Cl2); merging organic phases; carrying out reduced pressure distillation; removing a solvent to obtain a 1-methyl-3,4-binitro pyrromonazole product. The preparation method disclosed by the invention has the advantages of safety and low toxin content of the raw materials, simple synthetic process, high yield and high purity of products and easiness for industrialization.

Description

technical field [0001] The invention relates to a method for preparing 1-methyl-3,4-dinitropyrazole. The 1-methyl-3,4-dinitropyrazole prepared by the invention is high-energy insensitive and has a low melting point. It is a room temperature liquid explosive. technical background [0002] 1-Methyl-3,4-dinitropyrazole is a typical nitrogen-heterocyclic energetic compound. Because the pyrazole ring contains high-enthalpy C=C double bonds and N-N single bonds, it provides an opportunity to increase the enthalpy of formation. Conditions, therefore, nitrogen heterocyclic energetic compounds have the characteristics of high formation enthalpy, high density and environmental friendliness, have very considerable energy, and have good prospects in the fields of high-energy explosives, safety insensitivity, low-sensitivity additives, etc. . [0003] M.Ross Grimmett et al. (Ross Grimmett M, Richard Lim K H, Dinitration of l-methylpyrazole: l-methyl-3,4-dinitropyrazole. Aust J Chem, 19...

Claims

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Application Information

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IPC IPC(8): C07D231/16
Inventor 李永祥曹端林王建龙李雅津沈勇王艳红陈丽珍马忠平陈芳
Owner ZHONGBEI UNIV
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