Check patentability & draft patents in minutes with Patsnap Eureka AI!

A kind of synthetic method of methylnitrosamine

A synthetic method and technology of metronitramine, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as complex reaction steps, low yield, harsh hydrolysis conditions, etc.

Active Publication Date: 2021-02-26
XIAN MODERN CHEM RES INST
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the deficiencies and defects such as complicated reaction operation steps, harsh hydrolysis conditions, and low yield in the preparation process of metronitramine in the background technology, and provide a method for post-treatment operation that is simple and convenient, with mild hydrolysis conditions and low yield. Higher synthesis method of methylnitroamine

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Dissolve 100g of N,N'-dimethylurea in 200mL of dichloromethane to prepare a solution, and slowly add it to a mixed acid consisting of 278g of concentrated nitric acid with a mass concentration of 98% and 233g of concentrated sulfuric acid with a mass concentration of 98% for nitration reaction , The reaction temperature is -5°C to 0°C. After the addition is complete, the reaction mixture is poured into 400 g of ice water for dilution.

[0016] The diluent was heated to 20°C for hydrolysis reaction. The hydrolysis time was 60 minutes. After the reaction was terminated, the hydrolyzed liquid phase was separated, and the dichloromethane phase was dried with anhydrous magnesium sulfate and concentrated to obtain 150 g of metronitroamine with a yield of 86.9%. ≥99.3%.

[0017] Structural Identification of Metronitramine:

[0018] Elemental Analysis:CH 4 N 2 o 2 , calculated: C 15.79, H 5.263, N 36.84;

[0019] Found: C 16.16, H 5.312, N 37.28.

[0020] IR(KBr),υ / cm -1...

Embodiment 2

[0024] Dissolve 100g of N,N'-dimethylurea in 200mL of dichloromethane to prepare a solution, slowly add it to a mixed acid consisting of 201g of concentrated nitric acid with a mass concentration of 98% and 169g of concentrated sulfuric acid with a mass concentration of 98% for nitration reaction , The reaction temperature is -5°C to 0°C. After the addition is complete, the reaction mixture is poured into 400 g of ice water for dilution.

[0025] The diluted solution was heated to 5°C for hydrolysis reaction. The hydrolysis time was 30 minutes. After the reaction was terminated, the hydrolyzed liquid phase was separated, and the dichloromethane phase was dried with anhydrous magnesium sulfate and concentrated to obtain 115 g of metronitroamine with a yield of 66.6%. ≥98.9%.

Embodiment 3

[0027] Dissolve 100g of N,N'-dimethylurea in 200mL of dichloromethane to prepare a solution, and slowly add it to a mixed acid consisting of 260g of concentrated nitric acid with a mass concentration of 98% and 218g of concentrated sulfuric acid with a mass concentration of 98% for nitration reaction , The reaction temperature is -5°C to 0°C. After the addition is complete, the reaction mixture is poured into 400 g of ice water for dilution.

[0028] The diluent was heated to 25°C for hydrolysis reaction. The hydrolysis time was 80 minutes. After the reaction was terminated, the hydrolyzed liquid phase was separated, and the dichloromethane phase was dried with anhydrous magnesium sulfate and concentrated to obtain 146 g of metronitroamine with a yield of 84.5%. ≥98.6%.

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 method for synthesizing metronitramine. The method uses N,N'-dimethylurea as a raw material and comprises the following steps: (1) dissolving N,N'-dimethylurea in dichloromethane to prepare into a solution, slowly added to nitric acid mixed acid to carry out nitration reaction, the reaction temperature -5 ° C ~ 0 ° C, after the addition, the reaction mixture is poured into ice water for dilution; (2) the dilution obtained in the above (1) is warmed up to The hydrolysis reaction is carried out at 5°C to 30°C, and the hydrolysis time is 30min to 120min. After the reaction is terminated, the hydrolyzed liquid phase is separated, and the dichloromethane phase is dried with anhydrous magnesium sulfate, and then concentrated to obtain metronidamine. The invention aims to solve the problems of complex reaction operation steps, harsh hydrolysis conditions, low yield and the like in the preparation process of metronitramine. It is mainly used in the preparation of methylnitrosamine.

Description

technical field [0001] The invention relates to the nitration and hydrolysis of N,N'-dimethylurea, specifically a method for synthesizing metronitramine, which belongs to organic synthesis. Background technique [0002] Metronitroamine is an important organic compound, which can be used not only as a simple substance explosive, but also as an intermediate for the synthesis of nitramine energetic materials. [0003] The synthesis method of metronitramine is mainly based on N,N'-dimethylurea as raw material, first synthesize N,N'-dimethyl-N,N'-dinitrourea, and then carry out hydrolysis reaction to obtain the target things. U.S. Patents US4418212A and US4476322A disclose a method for synthesizing metronitroamine. N,N'-dimethylurea is dissolved in dichloromethane to prepare a solution, and nitric acid mixed acid is added for nitration. After the reaction is completed, pour ice water and use Extracted with dichloromethane, washed with alkali and water to obtain a dichloromethan...

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): C07C243/02C07C275/68C07C273/18
CPCC07C243/02C07C273/1863C07C275/68
Inventor 陈斌汪营磊刘亚静陆婷婷闫峥峰
Owner XIAN MODERN CHEM RES INST
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com