The method of obtaining trinational the salt postemergency acid uranyl

 

(57) Abstract:

The invention relates to the field of chemistry of organophosphorus compounds, in particular to an improved method for producing trinational the salt postemergency acid uranyl, which is carried out by reaction of sililirovanie phosphorous acid hexamethyldisiloxane taken at 1.5 to 2.5-fold excess of the stoichiometric required to monochloramine, subsequent similarobama and alkylation of intermediate reaction products undergo simultaneous introduction into the reaction mass hexamethyldisilazane in number, comprising 75-95% of the stoichiometric required, and alkylphosphonate, and saponification of Trevira postemergency acid is carried out in two stages, with the first stage using 20-70% stoichiometric alkali necessary, and the remaining amount of alkali - at the second stage. Trinacria salt postemergency acid uranyl has antiviral properties and is used in medicine. The technical result is an increase in the yield of the final product and the degree of cleanliness that meets the requirements of Gastarbajteri requirements for substances for injection solutions.

From the eve of salt postemergency acid uranyl, with protivovirusnym action and used in medicine.

Famous for a large variety of methods for obtaining trinational the salt postemergency acid based on phosphorous acid and its various derivatives. So, as the original products were used trialkylphosphine (lk)3R, where Alk=C1-C4that have been transformed by the action of alkylaromatic in truefire postemergency acid, followed by hydrolysis with alkali in chinatravel salt (application Germany No. 3607445, 07 F 9/38, 1987). The main disadvantage of this method is the high cost and inaccessibility of the original phosphites for production in the enlarged scale.

Described in the literature, the method of obtaining the specified product from dietilfosfat converting it into sodium salt, carboxylation, and then alkylation of dimethylsulfate formed the salt dibutylethanolamine acid and its alkaline hydrolysis (GDR patent No. 251137, 07 F 9/40, 1987). However, the necessity of using in the process of metallic sodium, explosive and flammable organic solvents significantly limit the possibility of its application in industry.

A method of obtaining trinational Sality action hexamethyldisilazane (HMDS) at 130-160°C for 5-10 hours (GDR patent No. 215085, 07 F 9/40, 1984). The most important disadvantages of this method include high consumption of expensive HMDS and high energy intensity of the process.

The closest in technical essence to the new method is a known method of producing uranyl trinational the salt postemergency acid, selected as a prototype (patent RF № 2110521, 07 F 9/38, publ. 1998). Synthesis is carried out according to the scheme below by successive transformations of phosphorous acid by the action of the stoichiometric amount of hexamethyldisiloxane and 1.1-to 1.3-fold excess hexamethyldisilazane respectively monocell- (1) and bis(silyl)fosfat (2), which then reacts with alkylchlorosilanes in the presence hexamethyldisilazane education Trevira postemergency acid (3).

Last omelet aqueous solution of caustic soda.

The main disadvantage of the prototype is that synthesized this way the product is suitable only for use in ointments and creams, but cannot be used for the preparation of injectable medicines, because the transparency of its 2-4,5-percentage aqueous solutions do not meet the requirements of the doctor). The reason, apparently, is the presence of a crystalline product of the admixture of the water-insoluble hexamethyldisiloxane, because in the process of hydrolysis, crystallization drop-down product is in intensively mixed heterogeneous reaction mixture water - hexamethyldisiloxane that can be seen from reactions

In addition, the disadvantages of the prototype method should be attributed to its higher energy intensity, because chetyrehstoronny the process requires heating the first three stages, and at last fairly long intensive cooling self-heating during hydrolysis of the reaction mixture.

A new way to get trinational the salt postemergency acid uranyl carry out initial sellerbuyer phosphorous acid hexamethyldisiloxane taken at 1.5 to 2.5-fold excess of the stoichiometric required to monochloramine, and the subsequent sellerbuyer and alkylation of intermediate reaction products with the simultaneous introduction into the reaction mass hexamethyldisilazane in number, comprising 75-95% of the stoichiometric required, and alkylphosphonate and subsequent saponification oberhasli necessary alkali and the remaining quantity of alkali - in the second stage. Preferably the test repeated sililirovanie and alkylation at a temperature of 50-90°C., and the reaction of saponification of at 40-50°C in the first stage and at 40-90°C on the second.

The new method differs from the method-prototype quantities of the raw materials and the modes of implementation of individual stages. So, obtained in the first stage, monosilicic (1) turn in triavir (3) simultaneous introduction into the reaction mixture hexamethyldisilazane and alkylphosphonate instead of two successive stages to obtain di(silyl)phosphite (2) and then alkylation (method prototype).

It turned out that when conducting the process in this mode for complete conversion of monosilicide (1) triavir postemergency acid (3) just 75-95% of the stoichiometric amount hexamethyldisilazane that 20-50% less than used in the method prototype. Apparently, the presence in the reaction mixture of two reagents simultaneously occurring reactions sililirovanie and alkylation. Released ammonia and trimethylchlorosilane interact with each other with the formation of hexamethyldisilazane.

In addition, the saponification of Trevira (3) is carried out in two steps: n the and alkali, in the reaction mixture formed two layers - hexamethyldisiloxane and an aqueous solution of a mixture of mono - and Dimitrievich the salts alkyldiphenylamine acid.

These intermediate formed salts are soluble in water, making it easy to separate hexamethyldisiloxane. Using less than 20% of the total quantity of alkali leads to partial, with the longer standing the resulting aqueous solution to a complete decomposition of intermediates emitting CO2. The increase in the quantity of alkali (>70%) leads to the precipitation of poorly soluble in water trinational salt.

In the second stage separated from hexamethyldisiloxane the aqueous layer was treated with the remaining amount of alkali with the formation of crystalline trinational salt. This reaction proceeds with the self heating of the reaction mixture up to 60-90°C, which contributes to the full completion of the hydrolysis alkylcarboxylic group and without the cost of long-term cooling. It should be noted that the crystallization of the product in a homogeneous environment in the absence of hexamethyldisiloxane allows you to receive the product, the transparency of the aqueous solutions which meets the requirements of Gastarbajteri, vsledstie the salt postemergency acid according to the new method is 87-95%.

Thus, a new method of producing uranyl trinational the salt postemergency acid differs from the prototype:

- greater efficiency, thanks to the savings of 20-50% hexamethyldisilazane is the most expensive source of reagent, as well as reducing the cost of heating and long-term cooling of the reaction mixtures;

- greater efficiency, because it allows to obtain a final product with almost quantitative yields (12-20% higher than in the method-prototype) and degree of purity, it can be used for the preparation of injection solutions;

- greater adaptability by conducting the process in more mild conditions.

Below, the new method is illustrated by two examples, which does not limit the possibility of carrying out the method in other conditions that are within the scope of the claims specified by the claims.

Example 1. A mixture of 574 g (7.0 moles) of phosphorous acid and 1500 ml (7.0 moles) of hexamethyldisiloxane boil until then, until you cease to be allocated water, and then distilled off the excess hexamethyldisiloxane. VAT residue at 50°C is mixed with 904 g (5,6 mole) hexamethyldisilazane and 662 grams (7.0 moles) meillor°C. The resulting two-layer system is separated aqueous layer was mixed with 25% solution 896 g (22,4 mole) sodium hydroxide at 40°C. the precipitation is filtered off and recrystallized from water. The output of uranyl trinational the salt postemergency acid is 85% of theoretical calculation on the source of phosphorous acid.

Example 2. A mixture of 574 g (7.0 moles) of phosphorous acid and 1500 ml (7 moles) of hexamethyldisiloxane boil until then, until you cease to be allocated water, and then distilled off the excess hexamethyldisiloxane. VAT residue at 86°C is mixed with 904 g (5,6 mole) hexamethyldisilazane and 662 grams (7.0 moles) of methylchloroform, the mixture is heated at this temperature and treated with 25% aqueous solution of 224 g (5,6 mole) sodium hydroxide at 50°C. the Resulting two-layer system is separated aqueous layer was mixed with 25% solution 896 g (22,4 mole) sodium hydroxide at 90°C. the precipitation is filtered off and recrystallized from water. The output of uranyl trinational the salt postemergency acid is 95% of theoretical calculation on the source of phosphorous acid.

1. The method of obtaining trinational the salt postemergency acid uranyl by sellerbuyer phosphorous acid g is alchoholism and aqueous sodium hydroxide solution, characterized in that the initial similarobama phosphorous acid is carried hexamethyldisiloxane taken at 1.5 to 2.5-fold excess of the stoichiometric required to monochloramine, subsequent similarobama and alkylation of intermediate reaction products undergo simultaneous introduction into the reaction mass hexamethyldisilazane in number, comprising 75-95% of the stoichiometric required, and alkylphosphonate, and saponification of Trevira postemergency acid is carried out in two stages, with the first stage using 20-70% stoichiometric alkali necessary, and the remaining amount of alkali - at the second stage.

2. The method according to p. 1, characterized in that the process of simultaneous sililirovanie and alkylation is conducted preferably at a temperature of 50-90S.

3. The method according to p. 2, characterized in that the first stage of saponification is preferably carried out at 40-50C, and the second stage at 40-90S.

 

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