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1-nitro-3-trinitromethylpyrazole compound

A technology of methylpyrazole and trinitro, which is applied in the field of pyrazole compounds and can solve the problems of low energy level and low oxygen balance

Active Publication Date: 2020-07-17
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the compound has a lower oxygen balance and a lower energy level

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Synthesis of 3-formaldehyde oxime pyrazole

[0022] Add 0.83g (12mmol) of hydroxylamine hydrochloride, 0.98g (12mmol) of sodium acetate and 40ml of ethanol into a 100ml three-necked flask, add 0.96g (10mmol) of 3-formaldehyde pyrazole under stirring, heat up to 60°C, and react for 2h. After the reaction, a milky white turbid liquid was obtained, cooled to room temperature, filtered, and the filtrate was evaporated to dryness to obtain an oily viscous solid, which was dissolved in 50ml of water and extracted three times with 50ml of ethyl acetate. The organic phase was dried with anhydrous sodium sulfate, filtered, and the filtrate was evaporated. After drying, 0.93 g of a light yellow viscous solid was obtained, with a yield of 84.0%.

[0023] Structure Identification:

[0024] NMR spectrum: 1 H NMR (600MHz, dmso): δ11.65, 8.13, 7.65, 7.65, 7.63, 7.63, 7.54, 6.88, 6.88, 6.49, 6.49; 13 C NMR (151MHz, dmso): δ172.83, 170.89, 144.19, 142.62, 140.09, 138.70, 133.02, ...

Embodiment 2

[0040] (1) Synthesis of 3-formaldehyde oxime pyrazole

[0041] Add 1.25g (18mmol) of hydroxylamine hydrochloride, 1.47g (18mmol) of sodium acetate and 40ml of ethanol into a 100ml three-necked flask, add 0.96g (10mmol) of 3-formaldehydepyrazole under stirring, heat up to 50°C, and react for 2h. After the reaction, a milky white turbid liquid was obtained, cooled to room temperature, filtered, and the filtrate was evaporated to dryness to obtain an oily viscous solid, which was dissolved in 50ml of water and extracted three times with 50ml of ethyl acetate. The organic phase was dried with anhydrous sodium sulfate, filtered, and the filtrate was evaporated. After drying, 0.96 g of light yellow viscous solid was obtained, and the yield was 86.8%.

[0042] Structure Identification:

[0043] NMR spectrum: 1 H NMR (600MHz, dmso): δ11.65, 8.13, 7.65, 7.65, 7.63, 7.63, 7.54, 6.88, 6.88, 6.49, 6.49; 13 C NMR (151MHz, dmso): δ172.83, 170.89, 144.19, 142.62, 140.09, 138.70, 133.02, 1...

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Abstract

The invention discloses a 1-nitro-3-trinitro methyl pyrazol compound. A structural formula of the 1-nitro-3-trinitro methyl pyrazol compound is as shown in a formula (I): (shown in the specification).The 1-nitro-3-trinitro methyl pyrazol compound is mainly used in the field of energetic materials.

Description

technical field [0001] The invention relates to an energetic material, in particular to a pyrazole compound. Background technique [0002] In recent years, aza five-membered aromatic ring compounds have become a research hotspot in the field of energetic materials due to their high nitrogen content, large gas production, and clean detonation products. Among them, pyrazole is a five-membered heterocyclic compound containing two adjacent N atoms. Its structure contains high-energy N-N, C-N bonds and greater ring tension. Large π bonds similar to benzene rings can be formed in the system, making this Compounds have good thermal stability. There is a π-electron system in the pyrazole structure, and the ring is easy to undergo reactions such as electrophilic substitution. It is one of the ideal structural units for the design and synthesis of high-nitrogen energetic materials. Trinitromethyl is the oxygen-rich energetic group with the highest oxygen content. The introduction of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/12C06B25/34
CPCC06B25/34C07D231/12
Inventor 张义迎熊存良张红武朱勇庞思平
Owner XIAN MODERN CHEM RES INST
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