Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Synthesis method for 2,2,4,4,6,6-hexanitro-adamantane

A synthetic method, the technology of the six nitrate foundation, applied in chemical instruments and methods, the preparation of organic compounds, organic chemistry, etc., can solve the problems of many waste acids, long steps, low yield, etc., and achieve high reaction yield and low cost. Low, high yield effect

Inactive Publication Date: 2015-07-22
NANJING UNIV OF SCI & TECH
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction route has long steps, many waste acids, heavy pollution and low yield

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
  • Synthesis method for 2,2,4,4,6,6-hexanitro-adamantane
  • Synthesis method for 2,2,4,4,6,6-hexanitro-adamantane
  • Synthesis method for 2,2,4,4,6,6-hexanitro-adamantane

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0041] Preparation of Meerwein's ester

[0042]

Embodiment 1

[0044] Add 228mL (1.50mol) of diethyl malonate, 37.5g (1.25mol) of paraformaldehyde, and 200mL of toluene into a 500mL round-bottomed flask in turn, and add 4.2mL (0.038mol) of N-methylpiperazine while stirring, first React at 100°C for 8h, then at 120°C for 10h. The solvent was distilled off under reduced pressure to obtain a light yellow oily liquid, which was cooled to room temperature and set aside. Add 57.4g (1.06mol) of sodium methoxide into 400mL of anhydrous methanol, stir until completely dissolved, and after cooling to room temperature, add the light yellow oily liquid obtained above to it. After reflux at 65°C for 12 hours, a light yellow solid precipitated out. After cooling to room temperature, it was filtered with suction, and the filter cake was washed with a mixed solvent of ether and methanol to obtain a white solid. Dissolve the white solid in 500 mL of water, adjust the pH to 4-5 with 6 mol / L hydrochloric acid, precipitate a large amount of white solid, fil...

Embodiment 2

[0046] Only change the amount of paraformaldehyde in Example 1 to 31.5g (1.05mol), change the reaction to first react at 80°C for 9h, change the amount of sodium methoxide to 81.2g (1.50mol), and other operations are consistent with Example 1 . Obtain 80.8g Meerwein's ester, yield 56%.

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

No PUM Login to View More

Abstract

The invention discloses a synthesis method for 2,2,4,4,6,6-hexanitro-adamantane. According to the method, diethyl malonate is used as a raw material, and the steps of cyclization, ozonization and the like with complex aftertreatment and low yield in the traditional route are avoided by a new route; and in the new route, N2O5 is used as a nitration agent in a nitration step, and the advantages of fast reaction speed, easily-controlled reaction temperature, easily-separated products, high product purity, capacity of effectively reducing waste acid, and the like are achieved. The method is lower in cost, less in reaction pollution and higher in yield compared with the traditional route, the reaction yield is increased to 14% from 0.5% of the original route, and possibility is provided for industrialized production for 2,2,4,4,6,6-hexanitroadamantane.

Description

technical field [0001] The invention relates to a synthesis method of adamantane derivatives, in particular to a synthesis method of 2,2,4,4,6,6-hexanitroadamantane. Background technique [0002] Adamantane and its derivatives are an important class of organic cage compounds, which can be widely used in medicine, energetic materials, functional polymers and other fields. Among them, polynitroadamantane has the advantages of high energy and low sensitivity due to its highly symmetric molecular structure, and can be used in the fields of explosives, propellants, pyrotechnics and fuels, so its theoretical and experimental research has been highly valued by people. The energy and detonation performance of polynitroadamantane increases with the increase of the number of nitro groups it contains. The calculation results show that the detonation velocity of 2,2,4,4,6,6-hexanitroadamantane is about 8700m·s -1 , the detonation pressure is about 34.6GPa, it is a high-energy explosiv...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/05C07C201/10
Inventor 罗军凌亦飞张萍萍孙露任晓莉
Owner NANJING UNIV OF SCI & TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com