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

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...