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A kind of synthetic method of 1,1'-diamino-5,5'-bitetrazole

A synthesis method, the technology of bitetrazole, which is applied in the field of synthesis of 1,1'-diamino-5,5'-tetrazole, can solve the problem of low yield of bitetrazole, and achieve simple operation and reduced operation Process, high purity effect

Active Publication Date: 2022-03-15
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] This method has a low yield of 1,1'-diamino-5,5'-bistetrazole, only 10%, and is accompanied by isomer compound 1,2'-diamino-5,5'-bistetrazole Tetrazole, 8%; requires column chromatography to obtain the pure compound 1,1'-diamino-5,5'-bitetrazolium

Method used

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  • A kind of synthetic method of 1,1'-diamino-5,5'-bitetrazole
  • A kind of synthetic method of 1,1'-diamino-5,5'-bitetrazole
  • A kind of synthetic method of 1,1'-diamino-5,5'-bitetrazole

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Experimental program
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Effect test

Embodiment 1

[0025] Add 1.0g of 1,1'-dicarbamate-5,5'-bitetrazole to dissolve in 10ml of methanol, put the solution into a sealed tube (specifically, a sealed reaction kettle commonly used in the chemical industry), and then add 0.52 g NaOH, seal the sealed tube and place it in an oil bath, heat it to 156°C, and react for 10 hours; then cool down, pour the reaction solution into 30ml water, extract with 3×10ml ethyl acetate, and wash the organic layer with anhydrous NaOH 2 SO 4 After drying, the solvent was removed by rotary evaporation under reduced pressure to obtain 0.27 g of solid powder 1,1'-diamino-5,5'-bitetrazole, with a yield of 50% and a purity of 98.6% (HPLC).

[0026] Structure Identification:

[0027] Infrared Spectrum: IR(KBr,cm -1 )υ: 3443,3338,3321,3259,3173,1621,1409,1388,1277,1132,1034,991,959,924,667;

[0028] NMR spectrum: 13 C NMR (DMSO-d 6 ,125MHz), δ:141.62(2C); 1 H NMR (DMSO-d 6 ,500MHz), δ:7.44(2NH 2 );

[0029] Elemental analysis: Molecular formula C2H4N1...

Embodiment 2

[0033] Add 1.0g of 1,1'-dicarbamate-5,5'-bitetrazol to 10ml of methanol to dissolve, put the solution into a sealed tube, then add 0.72g of KOH to it, seal the sealed tube and put In an oil bath, heat to 150°C and react for 10 hours; then cool down, pour the reaction solution into 30ml of water, extract with 3×10ml of ethyl acetate, and wash the organic layer with anhydrous Na 2 SO 4 After drying, the solvent was removed by rotary evaporation under reduced pressure to obtain 0.23 g of solid powder 1,1'-diamino-5,5'-bitetrazole, with a yield of 43% and a purity of 97.6% (HPLC).

Embodiment 3

[0035] Add 1.0g of 1,1'-dicarbamate-5,5'-bitetrazol to 10ml of ethanol to dissolve, put the solution into a sealed tube, then add 0.72g of KOH to it, seal the sealed tube and put it into In an oil bath, heat to 153°C and react for 10 hours; then cool down, pour the reaction solution into 30ml of water, extract with 3×10ml of ethyl acetate, and wash the organic layer with anhydrous Na 2 SO 4 After drying, the solvent was removed by rotary evaporation under reduced pressure to obtain 0.25 g of solid powder 1,1'-diamino-5,5'-bitetrazole, with a yield of 47% and a purity of 93.2% (HPLC).

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Abstract

The invention discloses a method for synthesizing 1,1'-diamino-5,5'-bitetrazolium. The disclosed method comprises: preparing 1,1'-dicarbamate-5,5'-tetrazolol solution by reacting 1,1'-dicarbamate-5,5'-tetrazolyl alcohol solution in a sealed environment, at a temperature of 150°C-160°C and in the presence of a base catalyst. Diamino-5,5'-bistetrazole. It further includes: adding water to the cooled reaction solution, extracting and drying to obtain solid powder 1,1'-diamino-5,5'-bitetrazolium. The synthesis method of the invention has high product yield, high purity and simple operation, and is suitable for large-scale synthesis of high-purity 1,1'-diamino-5,5'-bistetrazole.

Description

technical field [0001] The invention belongs to the field of energetic materials, in particular to a method for synthesizing 1,1'-diamino-5,5'-bitetrazolium. Background technique [0002] High-nitrogen and total-nitrogen compounds are currently a hot topic in the field of energetic materials. According to literature reports, high-nitrogen and total-nitrogen compounds may have better performance in some aspects, but because there are few known and synthesized high-nitrogen compounds, and all-nitrogen compounds have not yet been fully synthesized, so the current high-nitrogen and The properties of total nitrogen compounds are still guessed or predicted by theoretical calculations, so it is very necessary to synthesize more samples of high nitrogen and total nitrogen compounds. [0003] 1,1'-diamino-5,5'-bitetrazol, as a typical representative of high-nitrogen compounds, was recognized by Klapoetke, Thomas M. et al in "Amination of energetic anions: high-performing energetic m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/04
CPCC07D257/04
Inventor 吴敏杰毕福强翟连杰姚冰洁王伯周葛忠学汪伟
Owner XIAN MODERN CHEM RES INST