5-(1'-methyl)hydrazinotetrazolium and its metal salt derivative

A technology of hydrazine tetrazole and metal salt, applied in the field of new chemical materials and preparation thereof, can solve the problems of dangerous operation, unstable structure, difficult synthesis and the like, and achieve the effects of easy operation, high product purity and good stability

Inactive Publication Date: 2012-12-19
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nitrogen-rich tetrazole compounds such as 1,5-diaminotetrazole and 5,5'-azobistetrazole are not easy to synthesize

Method used

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  • 5-(1'-methyl)hydrazinotetrazolium and its metal salt derivative

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1, 5-(1 ' -Methyl)hydrazinotetrazole

[0026] Put 4.00 g (38 mmol) of cyanogen bromide in the reaction flask, add 50 mL of acetonitrile, and stir to dissolve at 0 °C. Add 10.00 g (154 mmol) sodium azide solid, stir the reaction at 0 °C for 4 h, and filter. The filtrate was added dropwise to a 30 mL acetonitrile solution containing methylhydrazine (0.92 g, 20 mmol), stirred for 4 h, and filtered. The precipitate was dried in vacuo at 80 °C to obtain a white solid, namely 5-(1 ' -methyl)hydrazinotetrazole. Yield: 73%. Take a small amount of white solid and dissolve it in a small amount of acetonitrile, slowly cool and let it stand, and obtain colorless transparent flaky crystals after 1 day, which is 5-(1 ' -Methyl)hydrazinotetrazole crystals.

[0027] The reaction formula is: BrCN+NaN 3 +CH 3 NHNH 2 à [CH 3 N(NH 2 ) CN 4 H]

Embodiment 2

[0028] Embodiment 2, 5-(1 ' -Methyl)hydrazinotetrazole

[0029] Put 1.06 g (10 mmol) cyanogen bromide in the reaction flask, add 0.65 g (10 mmol) sodium azide solid, dissolve in 20 mL water, add methylhydrazine (0.46 g, 10 mmol ), and stirred for 1 h. After the reaction, the water was drained to obtain a white mixture, which was extracted three times with 10 mL of acetonitrile, and the filtrates were combined and dried in vacuo to obtain a white solid, namely 5-(1 ' -methyl)hydrazinotetrazole. Yield: 58%.

[0030] The reaction formula is: BrCN+NaN 3 +CH 3 NHNH 2 à [CH 3 N(NH2 ) CN 4 H]

Embodiment 3

[0031] Embodiment 3,5-(1 ' -Methyl)hydrazino tetrazolium lithium salt

[0032] 2.28 g (20 mmol) 5-(1 ' -Methyl)hydrazinotetrazole was dissolved in 20 mL of water, 20 mL of an aqueous solution containing an equimolar amount (0.84 g, 20 mmol) of lithium hydroxide hydrate was added, and the reaction was fully stirred for 1 h. The solution was spin-dried in vacuo at 80 °C to obtain a white solid, namely 5-(1 ' - Methyl)hydrazinotetrazole lithium salt. Yield: 99%.

[0033] The reaction formula is: LiOH + [CH 3 N(NH 2 ) CN 4 H] à Li + [CH 3 N(NH 2 ) CN 4 ] - + H 2 o

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Abstract

The invention discloses a novel tetrazolium compound and its metal salt derivative, and preparation methods of the above compounds, and belongs to the fields of novel chemical materials and preparation technologies thereof. 5-(1'-methyl)hydrazinotetrazolium is prepared through reacting a cyanogen halogenide with sodium azide in a solvent, and reacting the resultant mixed solution/filtrate with methylhydrazine in the solvent. The metal salt of the 5-(1'-methyl)hydrazinotetrazolium is obtained through reacting 5-(1'-methyl)hydrazinotetrazolium/sodium 5-(1'-methyl)hydrazinotetrazolium with a metal hydroxide/metal sulfate/metal nitrate in water. The 5-(1'-methyl)hydrazinotetrazolium and the 5-(1'-methyl)hydrazinotetrazolium metal salt derivative prepared in the invention have a high nitrogen content and a good stability, can be used in energetic materials, can have magnetic characteristics, and have the advantages of simple preparation process and high purity.

Description

technical field [0001] The present invention relates to a class of novel tetrazole compounds and metal salt derivatives thereof, in particular to a class of novel 5-(1'-methyl)hydrazine tetrazole and metal salt derivatives based on this tetrazole, and The preparation method relating to these compounds belongs to the technical field of new chemical materials and their preparation. Background technique [0002] The tetrazole compound is a five-membered nitrogen-rich heterocyclic compound composed of four nitrogen atoms and one carbon atom. Generally, the structure of the tetrazole compound is changed by changing the functional group connected to the carbon atom. Tetrazole compounds have gradually attracted people's attention in recent years due to their high nitrogen content, high coordination number, easy-to-control and design structure, and relative stability, and have been used to prepare adsorbents, catalysts, pharmaceutical intermediates, and optical materials. , magneti...

Claims

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Application Information

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IPC IPC(8): C07D257/06
Inventor 陶国宏
Owner SICHUAN UNIV
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