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Method for synthesizing 5-nitramino tetrazole

A technology of nitroamino group and amino group, applied in the field of chemical synthesis, can solve the problems such as difficult preparation of nitric acid, complicated process, difficult to handle by-products and the like

Inactive Publication Date: 2009-06-24
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has problems such as complicated process, many steps, long period, low yield, high toxicity of raw materials, difficult to handle by-products, and high cost.
Another synthetic method is to use 100% nitric acid to directly nitrate 5-aminotetrazole to generate the target product, but 100% nitric acid is not easy to obtain, and nitric acid is flammable, so this method is inappropriate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1) In a 50ml there-necked flask, add 6.0g of concentrated nitric acid with a concentration of 95%, and slowly add 20g of concentrated sulfuric acid with a concentration of 98%, at a rate of 1ml / min, and add 4.30g of 5-aminotetrakis (nitrogen) under stirring. Azole, the temperature is controlled at 10-15°C. After the addition was complete, return to room temperature and continue stirring for 30 min.

[0015] 2) Slowly add 21.2 g of sodium carbonate to the above reaction solution at a rate of 2.12 g / min, and raise the temperature to 40° C. for 30 min.

[0016] 3) the mixture is naturally cooled to room temperature, washed 8 times with 100ml ethyl acetate, and filtered to obtain a white solid (Na 2 SO 4 ·xH 2 O) and 100ml ethyl acetate solution.

[0017] 4) The ethyl acetate solution was evaporated to dryness at 40° C. to obtain a white solid. Add 60 g of benzene to wash 6 times, and filter to obtain 4.8 g of white solid, which is pure 5-nitroaminotetra(az)azole, with...

Embodiment 2

[0019] 1) In a 50ml there-necked flask, add 6.0g of concentrated nitric acid with a concentration of 95%, and slowly add 10g of concentrated sulfuric acid with a concentration of 98%, at a rate of 1ml / min, and add 4.30g of 5-aminotetrakis (nitrogen) under stirring. Azole, the temperature is controlled at 10-15°C. After the addition was complete, return to room temperature and continue stirring for 30 min.

[0020] 2) Slowly add 39.4 g of barium carbonate to the above reaction solution at a rate of 2.12 g / min, and raise the temperature to 40° C. for 30 min.

[0021] 3) The mixture was naturally cooled to room temperature, washed 20 times with 200ml ethyl acetate, and filtered to obtain a white solid BaSO 4 and 200ml ethyl acetate solution.

[0022] 4) The ethyl acetate solution was evaporated to dryness at 40° C. to obtain a white solid. Add 60 g of benzene to wash 6 times, and filter to obtain 4.0 g of white solid, which is pure 5-nitroaminotetra(az)azole, with a yield of 6...

Embodiment 3

[0024] 1) In a 50ml there-necked flask, add 6.0g of concentrated nitric acid with a concentration of 95%, and slowly add 20g of concentrated sulfuric acid with a concentration of 98%, at a rate of 1ml / min, and add 4.30g of 5-aminotetrakis (nitrogen) under stirring. Azole, the temperature is controlled at 10-15°C. After the addition was complete, return to room temperature and continue stirring for 30 min.

[0025] 2) Slowly add 21.2 g of sodium carbonate to the above reaction solution at a rate of 2.12 g / min, and raise the temperature to 40° C. for 30 min.

[0026] 3) The mixture is naturally cooled to room temperature, washed 8 times with 100ml ether, filtered to obtain a white solid (Na 2 SO 4 ·xH 2 O) and 100ml ether solution.

[0027] 4) The diethyl ether solution was evaporated to dryness at 40°C to obtain a white solid. Add 60 g of benzene to wash 6 times, and filter to obtain 5.3 g of white solid, which is pure 5-nitroaminotetra(az)azole, with a yield of 81.5%.

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PUM

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Abstract

The invention relates to a synthetic method of 5-nitraminotetrazole, and belongs to the chemical synthesis field. The synthetic method comprises the following steps: firstly, nitrifying 5-aminotetrazole by a mixture of nitric acid and sulfuric acid; and then neutralizing excessive acid by alkaline substances such as sodium carbonate and the like; finally, purifying the 5-nitraminotetrazole by an organic solvent to obtain the purified 5-nitraminotetrazole. The synthetic method has the advantages of safe and reasonable process, short reaction time, simple steps, high yield, low production cost, no application and production of toxic substance, and simpler post-processing process.

Description

technical field [0001] The invention relates to a method for synthesizing 5-nitroaminotetrazole, which belongs to the field of chemical synthesis. Background technique [0002] 5-Nitraminotetra(nitrogen)azole, as a high-energy and low-sensitivity energetic compound, has a high N content, and its aromatic structure leads to its low sensitivity and good thermal stability. 5-Nitraminotetra(nitrogen)azoles can be used as components of airbags, ligands of new ionic salts (liquids), and explosives. The disclosed synthetic method of 5-nitroaminotetra(nitrogen)azole mainly takes 5-aminotetra(nitrogen)azole as raw material, adds nitric acid to generate nitrate, then adds concentrated sulfuric acid for dehydration, then adds barium carbonate to neutralize excessive Sulfuric acid to obtain white solid barium sulfate and aqueous solution, extract the aqueous solution with ether, evaporate the ether solution to dryness, add benzene to wash, and use 1,4-dioxane for recrystallization to o...

Claims

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Application Information

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IPC IPC(8): C07D257/06
Inventor 庞思平孙睿李玉川
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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