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Pentazole composite salt and preparation method thereof

A compound salt and phenyl pentazole technology, applied in the direction of organic chemistry, to achieve the effect of huge application value

Active Publication Date: 2017-03-22
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, due to the N 5 - Synthesis of technical difficulties, existing literature reportsN 5 - There are very few successful synthesis, and there is no successful synthesis of N that can exist stably at room temperature. 5 - report on compound salt

Method used

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  • Pentazole composite salt and preparation method thereof
  • Pentazole composite salt and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] In a single-necked flask, 4-hydroxyphenylpentazole (3mmol) was dissolved in a mixed solvent of methanol and acetonitrile (v / v, 1 / 1), and under the reaction condition of -45°C, ferrous glycinate (6mmol) was added Aqueous methanol (v / v, 1 / 4) (pre-cooled to -45°C), stirred for 30min, then added m-chloroperoxybenzoic acid (12mmol) in methanol (precooled to -45°C), reacted for 36h. Filtrate, remove most of the solvent by rotary evaporation, dissolve the obtained product in ethyl acetate, add water for liquid extraction, combine the water phases, and rotary evaporate through the column to obtain 21.2 mg of pentazole compound salt, with a yield of 12.08%.

Embodiment 2

[0033]In a one-necked flask, dissolve 4-hydroxyphenylpentazole (3mmol) in a mixed solvent of methanol and acetonitrile (v / v, 1 / 1), and add ferrous sulfate heptahydrate (6mmol) under the reaction condition of -45°C ) in methanol aqueous solution (v / v, 1 / 5) (pre-cooled to -45°C), stirred for 30min, then added m-chloroperoxybenzoic acid (12mmol) in methanol solution (pre-cooled to -45°C), and reacted for 36h . Filtrate, remove most of the solvent by rotary evaporation, dissolve the obtained product in ether, add water for liquid extraction, combine the water phases, and rotary evaporate through the column to obtain 14.5 mg of pentazole compound salt, with a yield of 8.26%.

Embodiment 3

[0035] In a single-necked flask, 4-hydroxyphenylpentazole (3mmol) was dissolved in a mixed solvent of methanol and acetonitrile (v / v, 1 / 1), and under the reaction condition of -45°C, ferrous chloride tetrahydrate ( 6mmol) of methanol aqueous solution (v / v, 1 / 6) (pre-cooled to -45°C), stirred for 30min, then added m-chloroperoxybenzoic acid (12mmol) in methanol solution (pre-cooled to -45°C), and reacted 36h. Filtrate, remove most of the solvent by rotary evaporation, dissolve the obtained product in ethyl acetate, add water for liquid extraction, combine the aqueous phases, and rotary evaporate through the column to obtain 12.5 mg of pentazole compound salt with a yield of 7.12%.

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Abstract

The invention discloses a pentazole composite salt and a preparation method thereof. By cutting off a C-N bond of substituted phenyl pentazole, a pentazolate anion is prepared. By adopting m-chloroperoxybenzoic acid and a ferrous salt as an oxidizing agent and a protective agent, respectively, a pentazolate-anion-containing composite salt [(N5)6(H3O)3(NH4)4Cl] is prepared. According to the invention, the pentazolate-anion-containing composite salt is achieved by cutting off the C-N bond of the substituted phenyl pentazole and successfully separating out the pentazolate anion. Also the synthesized pentazole composite salt can stably exist at normal temperature, and has great application values in the field of energetic materials.

Description

technical field [0001] The present invention relates to a kind of pentazole compound salt and preparation method thereof, be specifically related to a kind of compound salt containing pentazole anion [(N 5 ) 6 (H 3 O) 3 (NH 4 ) 4 Cl] and a preparation method thereof belong to the technical field of energetic materials. Background technique [0002] Due to the significant advantages of total nitrogen compounds in detonation performance over traditional energetic materials, the research focus in the field of energetic materials at home and abroad is gradually shifting from traditional energetic materials to new total nitrogen compounds. The most notable feature of all nitrogen compounds is that the molecule contains a large number of N-N and N=N bonds, which will release huge energy during the process of decomposing into nitrogen gas, and because the electronegativity of nitrogen is second only to F and O elements, It can form stronger chemical bonds, that is, the all-ni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D259/00
CPCC07D259/00
Inventor 胡炳成章冲余传明刘成
Owner NANJING UNIV OF SCI & TECH
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