Perdeuterated 2, 4-dinitroanisole and preparation method thereof

A technology of dinitroanisole and deuterated anisole, which is applied in the field of synthesis of deuterated energetic materials, can solve the problems that are unfavorable to industrial operation, unfavorable to industrial production, long reaction cycle, etc.

Active Publication Date: 2020-09-11
BEIJING INSTITUTE OF TECHNOLOGYGY
View PDF9 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2010, people such as Xia Xiaozhong used 2,4-dinitrobenzene as a raw material and synthesized 2,4-dinitroanisole with benzyltriethylammonium chloride as a phase transfer catalyst; although this method obtained 2, 4-Dinitroanisole, but the phase transfer catalyst is not easy to prepare, the cost is relatively high, and it is not suitable for large-scale use
In 2016, Liu Yan et al. used 1-chloro-2,4-dinitrobenzene (CDNB) as the raw material and KOH solution as the reaction medium to synthesize 2,4-dinitrobenzene in the next step without using a phase transfer catalyst. Anisole (Synthetic Chemistry, 2016,24(10):907-910); the optimal synthesis temperature range

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Perdeuterated 2, 4-dinitroanisole and preparation method thereof
  • Perdeuterated 2, 4-dinitroanisole and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A pressure vessel with a volume of 50 mL and filled with 6.5 g of deuterated acetic anhydride and 51 g of carbon tetrachloride was placed in a high-precision medium-temperature circulating bath at -5 °C, and was poured through a constant-pressure dropping funnel at a rate of 0.5 mL / min. Add deuterated nitric acid with a concentration of 98% in the container dropwise, and mechanically stir at a rate of 150 rpm while adding drops, and keep the temperature of the mixed solution not higher than 5°C. After 28 minutes, the dropwise addition is completed, and the temperature of the mixed solution is raised to 30°C. ℃; slowly add 2.3g of deuterated anisole into the mixed solution in 4 batches, maintain the temperature of the mixed solution at 30℃±0.5℃ during the addition process, then add 0.23g of sodium nitrate, after the addition is completed, seal the reaction device and increase Stirring rate to 400rpm, heat preservation for 4 hours, pour the mixture into 10mL deionized wate...

Embodiment 2

[0026] Place a pressure-resistant container with a volume of 100 mL and filled with 20.5 g of deuterated acetic anhydride and 175 g of carbon tetrachloride in a high-precision medium-temperature circulating bath at -5°C, and inject the Add deuterated nitric acid with a concentration of 95% in the medium dropwise, and mechanically stir at a rate of 150 rpm while adding drops, and keep the temperature of the mixed solution not higher than 5°C. After 51 minutes, the dropwise addition is completed, and the temperature of the mixed solution is raised to 25°C ; Slowly add 8.4g of deuterated anisole into the mixed solution in 6 batches, maintain the temperature of the mixed solution at 25°C ± 0.5°C during the addition process, then add 0.84g of potassium nitrate, after the addition, seal the reaction device and increase the stirring Speed ​​up to 400rpm, keep warm for 4 hours, pour the mixture into 25mL of deionized water at 5°C, stir at 50rpm for 1 hour, filter with suction, wash the...

Embodiment 3

[0029] Place a pressure-resistant container with a volume of 100 mL and filled with 23.5 g of deuterated propionic anhydride and 190 g of carbon tetrachloride in a high-precision medium-temperature circulating bath at -5°C, and inject the Add deuterated nitric acid with a concentration of 98% in the medium dropwise, and mechanically stir at a rate of 200 rpm while adding drops, and keep the temperature of the mixed solution not higher than 5°C. After 36 minutes, the dropwise addition is completed, and the temperature of the mixed solution is raised to 25°C ;Add 6.5g of deuterated anisole slowly to the mixed solution in 5 batches, maintain the temperature of the mixed solution at 25°C±0.5°C during the addition process, then add 0.654g of nickel nitrate, after the addition, seal the reaction device and increase the stirring Speed ​​up to 400rpm, keep warm for 5 hours, pour the mixture into 20mL of deionized water at 5°C, stir at 50rpm for 0.5 hours, filter with suction, wash the ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Crystal densityaaaaaaaaaa
Crystal densityaaaaaaaaaa
Hotaaaaaaaaaa
Login to view more

Abstract

The invention relates to perdeuterated 2, 4-dinitroanisole and a preparation method thereof, and belongs to the technical field of synthesis of deuterated energetic materials. Deuterated anisole is used as a raw material, and the raw material is relatively easy to obtain; the crude product only needs one purification step, the purity of the obtained product is high, and a standard solution for analysis can be directly prepared to serve as a deuterated internal standard substance for researching the metabolic process. Compared with common 2,4-dinitroanisole, the perdeuterated 2,4-dinitroanisoleprovided by the invention has the advantages that the crystal density is increased; meanwhile, the explosion heat is also increased. The perdeuterated 2,4-dinitroanisole can be used as an insensitivefusion casting carrier explosive, and the solubility of the sample to hexogen at 100 DEG C is increased to 17 g of hexogen dissolved in every 100 g of perdeuterated 2,4-dinitroanisole. The method isrelatively simple to operate, relatively short in reaction period and relatively high in product purity and yield, the preparation of the perdeuterated 2,4-dinitroanisole is realized, and a referenceis provided for industrial production of the perdeuterated 2,4-dinitroanisole.

Description

technical field [0001] The invention relates to a fully deuterated 2,4-dinitroanisole and a preparation method thereof, belonging to the technical field of synthesis of deuterated energetic materials. Background technique [0002] 2,4-Dinitroanisole is currently the most researched insensitive melt-cast carrier explosive, and it has received widespread attention since it came out in 1849. Compared with the common melting and casting explosive TNT, the shock wave sensitivity and thermal sensitivity of 2,4-dinitroanisole are relatively low. After melting and casting, the mechanical properties of the explosive are relatively ideal, the elasticity and toughness are good, the strength is high, and it is not easy to appear inside cracking etc. Moreover, 2,4-dinitroanisole is also an important chemical dye intermediate for the production of scarlet base RC (2-methoxy-5-nitroaniline hydrochloride). In addition, 2,4-dinitroanisole can also be used as an insecticide with excellent p...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C201/08C07C205/37C07C201/12C07C201/16
CPCC07B2200/05C07C201/08C07C201/12C07C201/16C07C205/37
Inventor 刘吉平方祝青
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap