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Preparation method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide

A technology of dinitropyridine and diaminopyridine, applied in the field of explosive synthesis, can solve the problems of difficulty in realizing industrialization, multiple impurities, high cost, etc., and achieve the effects of simple product post-processing, simplified process flow, and reduced production cost.

Inactive Publication Date: 2010-06-16
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although foreign researchers have vague and simple reports on this class of compounds (see: Hollins R, et al, J Heterocycl Chem, 1996, 33: 896-904), its synthetic route (see the figure below) and technology Determined that they can only be low yield (<50%), many impurities and high cost, it is difficult to realize industrialization

Method used

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  • Preparation method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide
  • Preparation method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide
  • Preparation method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide

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Embodiment 1

[0035] For the synthesis of 2,6-diacetylaminopyridine-1-oxide, the synthetic route is shown in accompanying drawing II. In a 100mL three-neck flask, add 5.45g (0.05mol) of 2,6-diaminopyridine, and add 33g of acetic anhydride dropwise while stirring; heat up to 45°C and continue the reaction for 1.5h. TLC detects that the basic reaction of the raw materials is complete, stop the reaction, and stir evenly . In the acetylation reaction solution, 0.079mol40% peracetic acid was added dropwise, reacted at 45°C for 2h, TLC detected that the raw materials had basically reacted completely, stopped the reaction, concentrated under reduced pressure, extracted three times with chloroform, combined organic phases and distilled to obtain 2,6- Diacetylaminopyridine nitrogen oxide crude product, yield 92%.

Embodiment 2

[0037] For the synthesis of 2,6-diacetylaminopyridine-1-oxide, the synthetic route is shown in accompanying drawing II. In a 100mL three-neck flask, add 5.45g (0.05mol) of 2,6-diaminopyridine, and add 33g of acetic anhydride dropwise while stirring; heat up to 45°C and continue the reaction for 1.5h. TLC detects that the basic reaction of the raw materials is complete, stop the reaction, and stir evenly . In the acetylation reaction solution, add 0.079mol40% peracetic acid and 0.5ml concentrated sulfuric acid dropwise, react at 45°C for 2h, TLC detects that the raw materials have basically reacted completely, stop the reaction, concentrate under reduced pressure, extract three times with chloroform, combine the organic phases and distill The crude product of 2,6-diacetylaminopyridine nitrogen oxide was obtained with a yield of 90%.

Embodiment 3

[0039] For the synthesis of 2,6-diacetylaminopyridine-1-oxide, the synthetic route is shown in accompanying drawing II. In a 100mL three-neck flask, add 5.45g (0.05mol) of 2,6-diaminopyridine, and add 33g of acetic anhydride dropwise while stirring; heat up to 45°C and continue the reaction for 1.5h. TLC detects that the basic reaction of the raw materials is complete, stop the reaction, and stir evenly . In the acetylation reaction liquid, add dropwise 0.079mol40% peracetic acid, 0.5ml concentrated sulfuric acid and 0.3g NaHSO 4 , reacted at 45° C. for 2 h, TLC detected that the reaction of the raw materials was basically complete, stopped the reaction, concentrated under reduced pressure, extracted three times with chloroform, combined organic phases and distilled to obtain crude 2,6-diacetylaminopyridine nitrogen oxide with a yield of 91.5%.

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Abstract

The invention relates to a preparation method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide. The method takes 2,6-diamino pyridine as a raw material; acyl group RCO-protection amino, peroxy acid R1COOOH / catalyst or sodium perborate oxidizing reaction realizes 2,6-diamino pyridine acylation and nitrogen oxidation reaction; a mixed acid or super acid nitrifying system is adopted to introduce nitryl on 3,5 site of 2,6-diacyl amino pyridine nitric oxide. The invention increases reaction safety, prevents nitrocompound from decomposing in the oxidation process and causes oxidation and subsequent nitratlon reaction to be easily carried out; in addition, the invention greatly lowers ubiquitous potential safety hazard in explosive synthesis, avoids use and maintenance of special equipment and devices and simplifies process flows; the invention has moderate reaction condition, does not need special devices, has abundant raw material resources, low cost, simple technology, safe and reliable production, simple product aftertreatment and small harm on environment, satisfies the basis requirements of industrial scale-up production.

Description

technical field [0001] The present invention relates to a kind of explosive synthesis technology, especially a kind of preparation high-energy insensitive explosive 2,6-diamino-3,5-dinitropyridine-1-oxide (2,6-diamino-3,5-dinitropyridine -1-oxide, abbreviated as: DADNPO) method. Background technique [0002] TATB (triaminotrinitrobenzene) is the most widely used high-energy heat-resistant explosive at home and abroad. Because of its extremely high tolerance to heat and mechanical action, it is favored in special fields such as missiles, rockets, aerospace and other military equipment, ultra-deep exploration seismic source bombs, and civilian blasting. However, TATB has high cost, high price (up to 2 million US dollars / ton), high pollution and high toxicity, which seriously limit its mass production and application. With the development trend of strengthening military industry and strengthening economy at home and abroad, people urgently need to develop some new high-energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89C06B25/34
Inventor 刘祖亮成健姚其正
Owner NANJING UNIV OF SCI & TECH
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