The method of producing uranyl trinational the salt postemergency acid

 

(57) Abstract:

The inventive product, the uranyl trinational the salt postemergency acid. Reagent 1: phosphoric acid. Reagent 2: hexamethyldisiloxane. Reagent 3: hexamethyldisilazane. The product of the interaction of reagents 1, 2 and 3 treated with alkylchlorosilanes, and then amyraut. Reaction conditions: heating to 100-120oC. 1 S. and 1 C.p. f-crystals.

The invention relates to the field of chemistry of organophosphorus compounds, in particular, to methods for producing uranyl trinational the salt postemergency acid, used in medicine and cosmetics as an anti-virus product.

Known methods for producing derivatives of postemergency acid, including its trinational salts of various organic and ORGANOMETALLIC compounds. So, as a starting product in the known method uses bimetallists and trimethylsilylmethyl (GDR patent N 215085, C 07 F 9/40, publ. 1984). The synthesis process in this case is carried out at 130-160oC for 4-10 hours the disadvantages of this method can be attributed to its high energy intensity and the inaccessibility of the original products. In another known method as ishodovanim metallic sodium in the presence of an anhydrous organic solvent (patent Spain N 556513, C 07 F 9/40, publ. 1985). These conditions of synthesis make an explosion and fire, limiting thus, the possibility of its industrial applications.

The closest in technical essence to the new method is a method of obtaining trinational the salt postemergency acid in the form of its uranyl, selected as a prototype (patent GDR N 243500, C 07 F 9/40, publ. 1987). In the way-the prototype of the synthesis process is carried out by a reaction between diapir phosphorous acid (a), Trevira phosphorous acid (b) with the ether Harborview acid (in) and hexamethyldisilazane (g) when the weight ratio is (a+b): = 10,33-10.5 and at 60-130oC, optimally at 80-110oC and subsequent saponification reaction mixture trialkylated ether postemergency acid and the esters trimethylsilylmethylamine acid with one or two siloxirane using sodium hydroxide, held first at 20-40oC, and then at 80oC for 2 hours All reactions in this way spend Paladino emitting intermediate products. The output of uranyl trinational the salt postemergency acid by the method prototype is 68,4% (based on ethyl ester postions, caused by the use of vacuum distillation for the separation of intermediate products - ethers with close boiling points: (MeO)2P(O)COOEt, (i-PrO)2P(O)COOEt, MeO(Me3SiO)P(O)COOEt, (ME3SiO)2P(O)COOEt. In addition, the implementation of the method prototype is quite time-consuming due to the harsh conditions of the implementation stage of hydrolysis of the mixture of esters with an aqueous solution of sodium hydroxide, and also due to the introduction stage acceleration difficult shared previously mentioned intermediate esters.

A new method to produce uranyl trinational the salt postemergency acid is carried sellerbuyer phosphorous acid in two stages: first, the stoichiometric quantity of hexamethyldisiloxane to education monocellular ester of phosphorous acid, and then the 1.1-to 1.3-fold excess of the stoichiometric amount hexamethyldisilazane to education disallowed ester of phosphorous acid by alkylation of the resulting product alkylchlorosilanes when heated and saponification of the resulting ester of postemergency acid aqueous solution of sodium hydroxide. Stage saponification, preferably, carried out at room temperature.

The new method offers Obedinenie in a new way selected phosphorous acid, which is the most readily available raw material for obtaining trinational the salt postemergency acid. It is introduced into the reaction sililirovanie in appropriate quantities based education intermediate - monocellular ester of phosphorous acid. As cilleruelo agent uses successively two connections: the first hexamethyldisiloxane, and then hexamethyldisilazane. Use exactly two similarbuy agents allows to carry out the reaction under mild conditions, namely when 90-120oC, and to make the process controlled without the desired emissions and losses to the original products. Of great importance is the sequence of similarbuy agents, namely first hexamethyldisiloxane, and then hexamethyldisilazane. In the case of using only hexamethyldisilazane process sililirovanie severely compromised. This is because the reaction hexamethyldisilazane with phosphorous acid along with monosilicide ammonia is formed, which, in turn, forms a crystalline acid ammonium salt, which leads to the formation of difficult to stir the mixture. In addition, this reaction is highly exothermic, which rubs disiloxane as cilleruelo agent of phosphorous acid, the process becomes manageable, as is carried out in a homogeneous medium at 90-100oC. Hexamethyldisiloxane is used in stoichiometric or near-stoichiometric quantities based education intermediate monosilicide. The end of the first stage of sililirovanie is determined by the completion of the selection of theoretical amount of water. After the first stage of distillation of unreacted hexamethyldisiloxane add the second similitude agent - hexamethyldisilazane that reacts with monosilicide to education sessilifolia. The second cilleruelo agent is a necessary condition for the entire process of sililirovanie, because the use of only one hexamethyldisiloxane leads to the formation of only monosilicide. For the introduction of the second trimethylsilyloxy group requires a stronger similarbuy agent, which is hexamethyldisilazane. This stage reaction is carried out at 100-120oC without complications. Hexamethyldisilazane at this stage is used in the 1.1-to 1.3-fold excess of the stoichiometric with respect to phosphorous acid, with hexamethyldisilazane in smaller quantities reaction sililirovanie not carried out, and ol the century

After the reaction of sililirovanie is the reaction of the alkylation reaction product. As alkylating product used alkylaromatic, such as methylchloroform, ethylchloride used in the 1.1 to 1.2-fold excess of the stoichiometric. Reducing the amount of alkylating agent below leads to a sharp decrease in the yield of the final product, and the overestimation of the quantity - to the formation of side products. The alkylation reaction is carried out at 60oC and after one-hour exposure is carried out stage saponification of the ester with an aqueous solution of caustic average concentration, such as 18-20%. The choice of alkali exactly the sodium hydroxide is explained by education trinational the salt postemergency acid. The process of saponification is carried out at room temperature, namely at 20-30oC, which is optimal at this stage. Last, the reaction may proceed at higher temperatures, however, with lower outputs. After adding sodium hydroxide solution, the reaction mass is then cooled to 5-10oC and incubated for 0.5 - 1 h and the precipitate is filtered off. The yield of the target product is 75% (based on the original factorystyle uranyl trinational the salt postemergency acid differs from prototype greater efficiency, as occurs with greater output, greater efficiency through the use of cheaper raw materials, higher intensity process, greater adaptability by conducting the process in more mild conditions

Example 1. To 180 g (2.2 mol) of phosphorous acid is added 500 ml of hexamethyldisiloxane. The resulting mixture is heated at 90-100oC for 1.5 h to water allocations. After heating of the reaction mass is distilled off unreacted hexamethyldisiloxane. To the mixture of reaction products at 70oC added dropwise with stirring 425 g (2.6 mol) hexamethyldisilazane, after which the mixture is heated to 100oC and kept at this temperature for 40 minutes Then the reaction product add to 228.7 g (2.4 mol) of methylchloroform and the reaction mass heated to 60oC and kept at this temperature for 1 h, then add 20% caustic soda solution of 37 g (1 mol). After cooling, the precipitate is filtered off. Output trinational the salt postemergency acid in the form of uranyl is 75% of theoretical calculation on the source of phosphorous acid.

Example 2. The process is carried out analogously to example 1, but with 2.2 mol of phosphorous acid, 500 M74%.

1. The method of producing uranyl trinational the salt postemergency acid sellerbuyer exitstrategy connection hexamethyldisilazane when heated, by alkylation of the resulting product alkylchlorosilanes when heated with subsequent saponification of the resulting Trevira postemergency acid aqueous solution of sodium hydroxide and isolation of the target product, characterized in that as exitstrategy connection using phosphorous acid and its sililirovanie additionally use hexamethyldisiloxane, and similarobama carried out in two consecutive steps: first the stoichiometric quantity of hexamethyldisiloxane to education monocellular ester of phosphorous acid, and then the 1.1 - to 1.3-fold excess of the stoichiometric amount hexamethyldisilazane to education disallowed ester of phosphorous acid.

2. The method according to p. 1, wherein the saponification is preferably carried out at room temperature.

 

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