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Synthesis method of 3,7-dinitro-1,3,5,7-4-azabicyclo[3,3,1]nonane

A technology of tetraazabicyclo and dinitro, applied in the field of synthesis of 3,7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane

Active Publication Date: 2012-07-04
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the yield of this method is low, and the highest yield in terms of urea is 60%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Add 13.6mL of 20% oleum to 17mL of 98% fuming nitric acid (density of 1.5g / mL) to prepare a mixed acid, and at a temperature of -5°C, add 6.0g of urea in batches to the above mixed acid, and stir 55min;

[0022] 2) Add the reaction solution of step (1) into 19.7mL ammonia solution with a temperature of -5°C and a concentration of 28%, adjust the temperature to 0°C-5°C, and keep stirring for 10 minutes;

[0023] 3) Add 40mL of 37% formaldehyde solution into the reaction solution in step (2), after the addition, raise the temperature to 40°C, stir for 10min, and then cool down to 25°C;

[0024] 4) Stirring at a temperature of 20°C, adding ammonia water with a concentration of 28% to the reaction solution of step (3), adjusting the pH of the reaction system to 7.2, during which precipitation is continuously precipitated, the precipitate is filtered, washed with water, and dried to obtain 3, 17.96 g of 7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane, with a yield of 75.4...

Embodiment 2

[0034] 1) Add 100mL 20% oleum to 140mL 98% fuming nitric acid (density 1.5g / mL) to prepare a mixed acid, add 60.0g urea in batches to the above mixed acid at a temperature of -5°C, and stir for 50min ;

[0035] 2) Add the reaction solution of step (1) into 168mL ammonia solution with a temperature of -5°C and a concentration of 28%, adjust the temperature to 0°C-5°C, and keep stirring for 20 minutes;

[0036] 3) Add 517mL of 37% formaldehyde solution into the reaction solution in step (2), after the addition, raise the temperature to 40°C, stir for 10min, and then cool down to 25°C;

[0037] 4) Under stirring, the temperature is 25°C, and the ammonia water with a concentration of 28% is added to the reaction solution of step (3), and the pH of the reaction system is adjusted to 7 with ammonia water, during which precipitates are continuously precipitated, filtered, washed with water, and dried to obtain 3 , 155.5 g of 7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane, with a yie...

Embodiment 3

[0039] 1) Add 750mL of 20% oleum to 625mL of 98% fuming nitric acid (density 1.5g / mL) to prepare a mixed acid, add 300g of urea in batches to the above mixed acid at a temperature of -5°C, and stir for 70min;

[0040] 2) Add the reaction liquid of step (1) into 1300mL ammonia solution with a temperature of -5°C and a concentration of 28%, adjust the temperature to 0°C-5°C, and keep stirring for 30min;

[0041] 3) Add 1620mL of 37% formaldehyde solution into the reaction solution in step (2), after the addition, heat up to 55°C, stir for 30min, and then cool down to 25°C;

[0042] 4) Under stirring, the temperature is 25°C, and the ammonia water with a concentration of 28% is added to the reaction solution of step (3), and the pH of the reaction system is adjusted to 7.5 with ammonia water, during which precipitation is continuously precipitated, the precipitate is filtered, washed with water, and dried to obtain 3 , 774 g of 7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane, and...

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Abstract

The invention discloses a synthesis method of 3,7-dinitro-1,3,5,7-4-azabicyclo[3,3,1]nonane, which comprises the following steps of: (1) adding 20% of fuming sulfuric acid to 98% of fuming nitric acid to prepare a mixed acid; adding urea in batches in the mixed acid at -5 DEG C and stirring for 40-90 min; (2) adding reaction liquid obtained in the step (1) in an ammonia spirit with the concentration of 28% and the temperature of -10-0 DEG C; and keeping the temperature at 0-5DEG C and stirring for 10-30 min; (3) adding 37% of formaldehyde solution in the reaction solution obtained in the step(2); and than raising the temperature to 40-65DEG C and stirring for 10-30 min; and then cooling to 20-25 DEG C, wherein the mole ratio of methanal and urea is 4.0-6.5:1.0; (4) adding ammonia spirit with the concentration of 28% in the reaction liquid obtained in the step (3) while keeping stirring; regulating the pH value of the reaction system to be 7-7.5 and regulating the temperature to be 20-25 DEG C; filtering and settling; washing with water and drying to obtain 3,7-dinitro-1,3,5,7-4-azabicyclo[3,3,1]nonane. The invention is mainly used for synthesizing 3,7-dinitro-1,3,5,7-4-azabicyclo[3,3,1]nonane.

Description

technical field [0001] The invention relates to a synthesis method of 3,7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane. Background technique [0002] 3,7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane is an intermediate for the preparation of eight-membered azacyclic ring nitramine compounds, and has a great potential in the field of organic synthesis important use. [0003] The method for synthesizing 3,7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane can use urea as a raw material. For example, "Chemistry of urea nitro derivatives: reaction of N, N'-dinitrourea with formaldehyde" Russian Journal of Organic Chemistry.2002, 38(12): 1739-1743 discloses a 3,7-dinitrourea-1,3,5 , Synthetic method of 7-tetraazabicyclo[3,3,1]nonane. The method uses urea as a raw material, and at a temperature of -5°C to 0°C, first add urea in batches to the mixed acid prepared by 20% oleum and 98% nitric acid, and stir for 30 minutes; pour the above reaction solution into crushed ice and stir vig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/08
Inventor 杨建明吕剑余秦伟刘波薛云娜谷玉杰葛忠学
Owner XIAN MODERN CHEM RES INST
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