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Synthetic method of 3-amino-4-hydroxyfurazan

A synthetic method and technology of hydroxyfuran, which is applied in the field of synthesis of 3-amino-4-hydroxyfuran, can solve the problems of low reaction yield, reduced reaction yield, increased by-products, etc., and achieve simple post-treatment process and high purity Good results

Inactive Publication Date: 2013-05-08
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the reaction yield of this method is low, and its reason is that the nitro group of 3-amino-4-nitrofurazan needs to be hydrolyzed by a strong base in the reaction process, although the nitro group can be hydrolyzed in a strong base environment It is a hydroxyl group, but it will also destroy part of the furoxan ring, resulting in an increase in by-products and reducing the yield of the reaction; It is obtained by oxidation, plus the synthesis of raw materials in one-step reaction, the method should undergo two-step reaction to obtain 3-amino-4-hydroxyfurazan

Method used

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  • Synthetic method of 3-amino-4-hydroxyfurazan
  • Synthetic method of 3-amino-4-hydroxyfurazan
  • Synthetic method of 3-amino-4-hydroxyfurazan

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Experimental program
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Effect test

Embodiment 1

[0020] 4g of 3,4-diaminofurazan and 45g of 24% (mass) sulfuric acid were added to the reaction flask under stirring, and at a temperature of -3°C to 3°C, 30mL of an aqueous solution containing 1.38g of sodium nitrite was added dropwise to the reaction flask. Control the dropping time for 2 hours. After adding the aqueous solution of sodium nitrite dropwise, react at a temperature of 0°C for 2 to 3 hours. At this time, the reaction liquid is pink; stop cooling and naturally heat up to 20°C to 25°C under stirring. Use a water bath to heat up to 50°C, and a large amount of nitrogen bubbles will emerge. After continuing to stir and react for 15 minutes, cool down in an ice-water bath to cool down to 0°C-5°C, stir for 30 minutes, and filter. The obtained filter cake is washed and vacuum-dried to After constant weight, 3.69 g of pale yellow-green solid 3-amino-4-hydroxyfurazan was obtained, with a yield of 91.4%.

[0021] Structure Identification:

[0022] Infrared (KBr, cm -1 ): ...

Embodiment 2

[0032] Add 4g of 3,4-diaminofurazan and 45g of 20% (mass) sulfuric acid into the reaction flask under stirring, and add 30mL of an aqueous solution containing 1.38g of sodium nitrite dropwise into the reaction flask at a temperature of -3°C to 3°C. Control the dropping time for 1.5h. After adding the aqueous solution of sodium nitrite dropwise, react at 0°C for 2-3h. At this time, the reaction liquid is pink; stop cooling and naturally heat up to 20°C-25°C under stirring. , use a water bath to heat up to 40°C, a large amount of nitrogen bubbles will emerge, continue to stir and react for 10 minutes, then cool down in an ice-water bath to cool down to 0°C-5°C, stir for 30 minutes, filter, and the obtained filter cake is washed and vacuum-dried After reaching a constant weight, 3.22 g of light yellow-green solid 3-amino-4-hydroxyfurazan was obtained, with a yield of 79.6%.

Embodiment 3

[0034] Add 4g of 3,4-diaminofurazan and 45g of 30% (mass) sulfuric acid into the reaction flask under stirring, and add 30mL of an aqueous solution containing 1.38g of sodium nitrite dropwise into the reaction flask at a temperature of -3°C to 3°C. Control the dropping time to 21.5 hours. After adding the aqueous solution of sodium nitrite dropwise, react at a temperature of 0°C for 2-3 hours. At this time, the reaction liquid is pink; stop cooling and naturally heat up to 20°C-25°C under stirring. , use a water bath to heat up to 40°C, a large amount of nitrogen bubbles will emerge, continue to stir and react for 30 minutes, then cool down in an ice-water bath to cool down to 0°C-5°C, stir for 30 minutes, filter, and the obtained filter cake is washed and vacuum-dried After reaching a constant weight, 3.38 g of light yellow-green solid 3-amino-4-hydroxyfurazan was obtained, with a yield of 83.7%.

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Abstract

The invention discloses a synthetic method of 3-amino-4-hydroxyfurazan. The structure of 3-amino-4-hydroxyfurazan is represented by a formula shown in the specification. The method which treats 3,4-diaminofurazan as a raw material comprises the following steps: adding 3,4-diaminofurazan and 20-30% (mass) sulfuric acid into a reaction bottle under stirring, adding an aqueous solution of sodium nitrite into the reaction bottle at -5-5DEG C in a dropwise manner under a condition that the addition time is controlled in a range of 1.5-2.5h, reacting at -5-5DEG C for 2-3h after the addition, naturally heating to 20-25DEG C under stirring, carrying out water-bath heating to 40-60DEG C, reacting for 10-20min, cooling to 0-5DEG C, stirring for 20-40min, filtering, washing the obtained filter cake, and drying to obtain 3-amino-4-hydroxyfurazan. The method is mainly used for preparing 3-amino-4-hydroxyfurazan.

Description

technical field [0001] The invention relates to a synthesis method of 3-amino-4-hydroxyfurazan. Background technique [0002] Furazan compounds have the characteristics of high energy and high density that energetic molecules should have. This is because the structure of furazan compounds contains a large number of C-O, C-N and N-N bonds, so their molecular chemical potential mainly comes from high formation enthalpy. Experiments have shown that most furoxan compounds are insensitive to static electricity, friction and impact. This is due to the high electronegativity of nitrogen and oxygen atoms in furazan high-nitrogen compounds, and their nitrogen-heteroaromatic ring systems can generally form benzene-like compounds. The large π bond of the structure has the properties of insensitivity and thermal stability. [0003] 3-Amino-4-hydroxyfurazan is a key intermediate in the synthesis of high-energy furazan-type energetic materials with high energy density. Its molecular stru...

Claims

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Application Information

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IPC IPC(8): C07D271/08
Inventor 郭涛雷鸣刘敏邱少君葛忠学姜俊唐望郑晓东李红丽秦明娜石强吕英迪陈志强张彦王子俊
Owner XIAN MODERN CHEM RES INST
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