SU1696426A1 - Method of 2 - Google Patents

Abstract

The invention relates to substituted ethylamines, in particular to the preparation of 2,2-dinitroethylamine, which can be used in the preparation of a number of polynitro compounds. The goal is to simplify and improve process safety, expanding the resource base. The preparation is carried out from 2,2,2-trinitroethanol acetate and an aqueous solution of formaldehyde in the presence of copper sulphate at 100-105 ° C for 7-8 hours. The intermediate is separated by solvent extraction. The solvent is removed, followed by treatment with ammonia for 25-30 ° C. 1 tab.

Description

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WITH

This invention relates to the chemistry of polyvitroalkylamines, in particular to an improved method for the preparation of 2,2-dinitroethylamine, which can be used as a starting material for the production of a number of polynitro compounds, for example, dipotassium salt 1, 1, 5, 5-tetra-nitro-3 α-azapentane, 1,1,5,5-tetranitro-3-nitroso-3-azapentane, 1,1,3,5,5-pentanitro-3-azo-pentane or 1,1,3,5,7,7 -hexanitro-1,5-diazacyclooctane.

He knows the method of producing 2,2-dinitroethylamine by acting on 1,1,1-trinitroethane at 35-40 ° C with gaseous ammonia in methanol medium. The yield of 2,2-dinitroethylamine is 83% 1.

The disadvantage of this method is the difficulty of obtaining the original 1.1,1-trinitroethane, which is synthesized from

explosive nitronate salts with a yield not exceeding 58% 2.

In view of the yield of the starting product, the yield of 2,2-dinitroethylamine is 48%.

The aim of the invention is to simplify and improve process safety, as well as expanding the resource base.

The goal is achieved by those. that 2,2,2-trinitroethanol acetate is reacted with an aqueous solution of formaldehyde in the presence of copper sulphate at 100-105 ° C for 7-8 h, the intermediate compound is isolated by solvent extraction, such as tributyl or tripropyl phosphate or dibutyl phthalate, the solvent is removed treated and then treated with gaseous ammonia in methanol at 25-30 ° C.

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Example: In a three-necked flask equipped with a mechanical stirrer with a hydraulic shutter, a thermometer and a reflux condenser, 60 ml (0.7 mol) of a 35% aqueous formaldehyde solution, 0.44 g (0.00176 mol) CuS04 5Н20 and 10 g are placed. (0.045 mol) acetate 2,2,2-tri-nitroethanol.

The reaction mixture is heated with stirring at a temperature of 100-101 ° C for 7 hours, then cooled to room temperature and extracted with tripropyl phosphate (2 x 20 ml). The solvent is distilled off under reduced pressure (1 mm Hg), the residue is dissolved in methanol and ammonia gas is passed through the resulting solution at 25-30 ° C. The yellow crystalline precipitate is filtered off and washed with ether. After drying in the air, 3.15 g of 2,2-dinitroethylamine was obtained. 123-124 ° C (decomp.) Yield 52%. 1 Calculated. %: C, 17.78; H 3.73; N 31.11.

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Found,%: C 18.00; H 3.5; N 31.5.

The data for examples 1-8 are presented in the table.

Thus, the proposed method eliminates the use of scarce raw materials - compounds of silver and iodine, replacing them with available raw materials - acetate.

2,2,2-trinitroethanol, formaldehyde, copper sulfate, and also improve working conditions by eliminating highly sensitive and explosive nitronate and silver salts of polynitroalkanes from the process.

Claims (1)

The invention The method of obtaining 2,2-dinitroethylamine, which includes the processing of polynitron compounds with gaseous ammonia in the environment methanol, characterized in that, in order to simplify and increase the safety of the process, expanding the raw material base, 2,2,2-trinitroethanol acetate is reacted with an aqueous solution of formaldehyde in the presence of copper sulphate at 100-105 ° C for 7-8 h, isolated The intermediate polynitro compound is extracted by solvent extraction, such as tributyl or tripropyl phosphate, or dibutyl phthalate. with the subsequent removal of the solvent and then treated with ammonia.