SU583124A1 - Method of preparing methylnitramine - Google Patents

Description

This invention relates to a process for the production of primary nitramines, in particular methylnitramine, which is used as the starting material for organic syntheses of products for various purposes. The method for producing methyl nitramide by nitration of K-methyl-1 -toluene sulfide with aaotic acid at a temperature, followed by purification of the obtained methyl nitramide, is known. p-topuolsulfonic acid b.p. an aqueous solution of caustic soda and processing the obtained salt with mineral acid. The yield of methylnitramine is 66%. The disadvantage of this method is the relatively low yield of the target product, the need to boil the reaction mass and the low availability of n-toluene sulfamide, the invention is the development of a more simple method of producing methylnitramine with a higher yield of the target product, Methylnitramine is obtained by treating C-methyl cyanethyl nitramine with caustic alkalis in a medium with a panic solvent at a temperature of 15-80 ° C, followed by separation of the target product by acidification with mineral acid. The starting N-methylanethenylnitramine is prepared by known methods from acrylonitrile and methylamine, followed by nitration of the nitrate salt / K-methyl cyanoethylamine with nitric acid. All reagents used for this purpose have an industrial base, are widely available. The addition of methylamine to acrylonitrile, the preparation of the nitrate salt of N-methnlycyanethylamine and the nitration of this SALT proceed easily and in high yields. Exit | -methyl cyanoethshitramine 9O-93% theoretical for methylamine and acrylonitrile. Pd decyanethylation. H-methylpianethylnitramine with anhydrous caustic alkalis or theirhydrous: and alcohol solutions in the medium of alcohols, acetone, dichloroethane, methylnitramine is released as insoluble salts in the reaction mass with a practically quantitative yield. The resulting methylnitramine salts can be easily filtered or converted to methylnitramine directly into the reaction.

mass by acidification with hydrochloric or once-Example 2. The synthesis is carried out as an sulfuric acid. Those formed in example 1, only the mixture is acidified with acid and precipitate: precipitate, they are stirred at a temperature of 10 ° -8 ° C and filtered, and ltilylnthramine is removed for 2 minutes and then cooled to a pure mixture by evaporation of the solvent. Output 5th air temperature. Similar results are obtained for methyln-fwmine 89 - 87 for C-methyldian-results, ethylnitramine n about 80% for the original methylamine. PrechmerZ. 129 g of methylnitramide is quite high (1 me) in the reactor at the mixing stage and 1 room temperature. , ZOOmp degree of chistegta (T. 36-38 C) and in most cases, 41H1, O25 mop) of the unit. The most cases can be used without a mixture that is stirred for 2 hours at a temp. Additional cleaning. 15-25 ° C and processed at temp. Example 1. In p The factor is loaded with pac-psure from -b to 5 concentrated consvor 129 VN {1 mol) M-methyldianethylnyl-p-5 acid (90.6 ml). Chloroyoramine precipitated in Zoo part of ethyl alcohol, 41 cb.h. the sodium is filtered off, the filtrate upar (1 O25 mol) of water is added and the reaction is carried out and metstnitramine is obtained. Exit the 63 g mixture is stirred at a temperature (85.5%). T ,, 36-38 С, 80-85Ч: (10mm), 15-25 С for 2 hours. The precipitate of sodium salt of methylnitramine is filtered, 20

the solvent is evaporated on dryness, the product Formulas of a-invention are combined, washed on a 40–5 O filter,

acetone is dried on waduah. Wyhpd 98 &. H. Method for the production of methylnitramine by

(1OO%) processing derivatives of methylnitramine shelo

Suspension 98 v.ch, (1 mol) | sodium salt, followed by isolation of the target

methylvitramin in 400 ob.h. chloride product, for example, by acidification with a solution

Lena is treated at a temperature of from -5 to; mineral acid, which differs from 5 ° C to 89 parts by volume concentrated hydrochloric acid in order to increase the yield

lots. The reaction mixture is stirred for 1 hour, the product and the procession proyessa, as

a solution of methylnitramine in methyl chloride derived from methylnitramine is taken AND -methyne is removed, dried with magnesium sulfate, cyanoethylnitramine and the process is carried out in a medium

the solvent is distilled off; Exit 69 v.ch. (91%) organic solvent at temperature

TjiV 36-38 S.. (About mm). .16 - 8O S.

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