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A kind of pyridofuroxan energetic compound and its preparation method

A technology of furoxan and compound, which is applied in organic chemistry and other fields, can solve the problems that the detonation performance of pyridine ring series energetic compounds cannot be fully utilized, and achieve the effects of small environmental hazards, mild conditions, and safe and reliable production

Active Publication Date: 2021-04-16
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The theoretically calculated detonation velocity of this compound is only 7.51km / s, which cannot give full play to the detonation performance of energetic compounds of the pyridine ring series

Method used

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  • A kind of pyridofuroxan energetic compound and its preparation method
  • A kind of pyridofuroxan energetic compound and its preparation method
  • A kind of pyridofuroxan energetic compound and its preparation method

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preparation example Construction

[0024] The preparation method of 4-amino-5-nitro-[1,2,5]oxadiazolo[3,4-e]tetrazol[1,5-a]pyridine-3-oxide of the present invention comprises the following steps :

[0025] In the first step, 4-amino-2,6-dichloro-3,5-dinitropyridine was dissolved in a suitable solvent, sodium azide was added at room temperature, and the reaction was stirred for 1 hour;

[0026] In the second step, a small amount of concentrated hydrochloric acid is added to the reaction mixture, and the temperature is raised to react for a period of time. After the reaction is completed, the mixture is evaporated under reduced pressure to remove the solvent, dissolved in water, extracted with ethyl acetate, dried on the organic phase, and distilled under reduced pressure to obtain 4-Amino-5-nitro-[1,2,5]oxadiazo[3,4-e]tetrazol[1,5-a]pyridine-3-oxide.

[0027] Wherein, in the first step, the molar ratio of 4-amino-2,6-dichloro-3,5-dinitropyridine to sodium azide is 1:2-1:4, which is used to dissolve 4-amino-2 ,...

Embodiment 1

[0030] Dissolve 1.26g (5mmol) of 4-amino-2,6-dichloro-3,5-dinitropyridine in 15mL of acetonitrile, add 0.65g (10mmol) of sodium azide under stirring at room temperature, and stir for 30min. 1 drop of concentrated hydrochloric acid was added to the reaction mixture, and the temperature was raised to 30° C. for 3 h. After the reaction, the mixed solution was rotary evaporated under reduced pressure, dissolved in water, extracted with ethyl acetate, the organic phase was dried and filtered, and the filtrate was distilled under reduced pressure to obtain a yellow solid 4-amino-5-nitro-[1,2,5]oxane Oxadiazo[3,4-e]tetrazol[1,5-a]pyridine-3-oxide 0.89 g, yield 75%. m.p.150-151℃(dec.); 1 H NMR (DMSO-d 6 ,400MHz):δ10.17(s,1H),9.50(s,1H); 13 C NMR (DMSO-d 6 ,100MHz): δ148.96, 144.27, 141.87, 111.17, 105.06; MS (ESI) m / z: 239.0 (M+H). See figure 1 .

[0031] The compound has the structures of tetrazole, furazan oxide and aminonitronitropyridine at the same time, and the theoretical...

Embodiment 2

[0033] Dissolve 1.26g (5mmol) of 4-amino-2,6-dichloro-3,5-dinitropyridine in 15mL of ethyl acetate and acetone mixed solvent, add 0.98g (15mmol) of azide under stirring at room temperature Sodium, stirred and reacted for 30min. Add 1 drop of concentrated hydrochloric acid to the reaction mixture, heat up to 35°C for 2.5h. After the reaction, the mixed solution was rotary evaporated under reduced pressure, dissolved in water, extracted with ethyl acetate, the organic phase was dried and filtered, and the filtrate was distilled under reduced pressure to obtain a yellow solid 4-amino-5-nitro-[1,2,5]oxane Oxadiazo[3,4-e]tetrazol[1,5-a]pyridine-3-oxide 0.71 g, yield 60%.

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Abstract

The invention discloses a pyridofurazan energetic compound and a preparation method thereof. The method is to realize the azidation and denitrification ring-closing reaction of 4-amino-2,6-dichloro-3,5-dinitropyridine at a certain temperature. After the reaction is completed, the mixture is rotated under reduced pressure and dissolved in water. , after extraction, the organic phase was dried with anhydrous sodium sulfate, filtered, and the filtrate was rotary evaporated under reduced pressure. The energetic compound synthesized by the invention has a novel structure, mild reaction conditions, no need for special equipment, simple process and operation process, safe and reliable production, convenient post-treatment of products, less environmental pollution, and meets the basic requirements of industrial scale-up production; the compound has both The structures of tetrazole, furazan oxide and aminonitropyridine have potential applications in the field of energetic materials, and the theoretically calculated detonation velocity reaches 8754 m / s.

Description

technical field [0001] The invention belongs to the technical field of explosive synthesis technology, in particular to an energetic compound 4-amino-5-nitro-[1,2,5]oxadiazole[3,4-e]tetrazole[1,5- a] Synthesis of pyridine-3-oxides. Background technique [0002] In the field of energetic materials, energetic derivatives with furazanyl oxide as the explosive group have the following characteristics: 1) furazanyl oxide can provide relatively higher energy density; 2) its effective oxygen content is high, and furazanyl oxide As energetic additives, the derivatives can improve the oxygen balance of the system; 3) Furazanyl oxide can endow the derivatives with ring tension and high standard enthalpy of formation. If a nitro group is replaced by a furazanyl oxide, the density can be increased by 0.06-0.08g / cm 3 , the detonation velocity can be increased by 300m / s. In addition, the introduction of the heterocyclic ring system can make the combination of atomic orbitals much bette...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/14
CPCC07D498/14
Inventor 马丛明刘祖亮姚其正周九九
Owner NANJING UNIV OF SCI & TECH
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