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Synthetic method of 3-azido-4-nitrofurazan

A technology of nitrofurazan and synthesis method, applied in the direction of organic chemistry, etc., can solve the problems of low reaction yield, cumbersome post-treatment, etc., and achieve the effect of complicated operation process

Active Publication Date: 2018-04-20
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction yield of this method is low and the post-treatment is cumbersome, and column chromatography purification is required to obtain the pure product of 3-azido-4-nitrofurazan

Method used

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  • Synthetic method of 3-azido-4-nitrofurazan

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Effect test

Embodiment 1

[0017] Stir at -5°C, add 3.0g of sodium tungstate to 28g of 50% hydrogen peroxide by mass percentage, then dropwise add 41g of 98% by mass sulfuric acid, react for 20min after the dropwise addition, and then add 1.0g of 3 -Azido-4-aminofurazan, after the addition, react at a temperature of 15°C for 4h, pour the reaction solution into ice water and extract with dichloromethane, dry the organic phase with anhydrous magnesium sulfate, filter and concentrate to obtain 3 -Azido-4-nitrofurazan 0.89g, yield 71.9%.

[0018] Infrared spectrum: IR (KBr) ν: 2150, 1536, 1485, 1378, 1355, 1181, 1021;

[0019] NMR spectrum: 13 C NMR (DMSO-d 6 ,125MHz), δ: 155.495,149.730;

[0020] MS (EI) m / z (%): 156 (M+, 1).

[0021] The above structural identification data confirm that the substance obtained in this step is indeed 3-azido-4-nitrofurazan.

Embodiment 2

[0023] Stir at 10°C, add 3.0g of sodium tungstate to 30g of 50% hydrogen peroxide by mass percentage, then dropwise add 41g of sulfuric acid with a mass percentage of 98%, react for 20 minutes after the dropwise addition, and then add 1.0g of 3- Azido-4-aminofurazan, after the addition, react at a temperature of 15°C for 4h, pour the reaction solution into ice water and extract with dichloromethane, dry the organic phase with anhydrous magnesium sulfate, filter and concentrate to obtain 3- Azido-4-nitrofurazan 0.90g, yield 72.7%.

Embodiment 3

[0025] Stir at 10°C, add 3.3g of sodium tungstate to 28g of 50% hydrogen peroxide by mass percentage, then dropwise add 50g of sulfuric acid with a mass percentage of 98%, react for 30min after the dropwise addition, and then add 1.0g of 3- Azido-4-aminofurazan, after the addition, react at a temperature of 20°C for 8h, pour the reaction solution into ice water and extract with dichloromethane, dry the organic phase with anhydrous magnesium sulfate, filter and concentrate to obtain 3- Azido-4-nitrofurazan 0.90g, yield 72.7%.

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Abstract

The invention discloses a synthesis method of 3-azido-4-nitro-furazan. The method comprises the following steps: adding sodium tungstate into 50 wt% oxydol at -5 to 15 DEG C while stirring, dropwisely adding 98 wt% sulfuric acid, reacting for 20-50 minutes after finishing the dropwise addition, adding 3-azido-4-aminofurazan at 10-20 DEG C, reacting at 15-25 DEG C for 4-10 hours after finishing charging, pouring the reaction solution into ice water, extracting with dichloromethane, drying the organic phase with anhydrous magnesium sulfate, filtering, and concentrating to obtain the 3-azido-4-nitro-furazan, wherein the mass ratio of the 3-azido-4-aminofurazan, oxydol, sulfuric acid and sodium tungstate is 1:(28-32):(41-66):(3.0-3.5).

Description

technical field [0001] The invention relates to a synthesis method of 3-azido-4-nitrofurazan, belonging to the field of energetic materials. Background technique [0002] As a basic structural unit, the furazan ring can construct a series of new energetic compounds with excellent performance. They generally have the advantages of high energy density, large standard enthalpy of formation, high nitrogen content, and good thermal stability, so they have become a large class of important compounds today. energetic materials. 3-azido-4-nitrofurazan calculated density 1.796g / cm 3 , The calculated enthalpy of formation is 535.4kJ / mol, the calculated detonation velocity is 8856m / s, and the calculated detonation pressure is 35.4GPa. It is not only an energetic compound with high energy, but also a compound for the synthesis of triazolofurazan, furazan ether and other compounds important intermediates, so in-depth study of its synthetic methods has a certain significance. For examp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D271/08
CPCC07D271/08
Inventor 王锡杰毕福强王伯周李祥志张俊林周诚霍欢
Owner XIAN MODERN CHEM RES INST