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Synthesis method of methyl-nitramine

A synthesis method and technology of metronidamine are applied in chemical instruments and methods, preparation of organic compounds, preparation of urea derivatives, etc., and can solve problems such as harsh hydrolysis conditions, low yield, and complicated reaction operation steps.

Active Publication Date: 2018-08-24
XIAN MODERN CHEM RES INST
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  • 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 proc

Method used

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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%.

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PUM

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Abstract

The invention discloses a synthesis method of methyl-nitramine. The method takes N,N'-dimethylurea as a raw material and comprises the following steps: (1) dissolving N,N'-dimethylurea into dichloromethane to prepare a solution; slowly adding the solution into mixed acid of nitric acid and sulfuric acid and carrying out nitration reaction, wherein the reaction temperature is -5 DEG C to 0 DEG C; after finishing charging, pouring a reaction mixture into ice water and diluting; (2) raising the temperature of a diluted solution obtained by step (1) to 5 DEG C to 30 DEG C and carrying out hydrolysis reaction, wherein the hydrolysis time is 30min to 120min; after stopping reaction, separating a hydrolysis liquid phase; after drying a dichloromethane phase through anhydrous magnesium sulfate, concentrating to obtain methyl-nitramine. According to the synthesis method, the problems of a methyl-nitramine preparation process that operation steps of the reaction are complicated, hydrolysis conditions are harsh, the yield is low and the like are solved; the synthesis method is mainly used for preparing methyl-nitramine.

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

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Application Information

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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
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