The method of producing uranyl trinitroresorcinate

 

(57) Abstract:

The inventive product, the uranyl trinitroresorcinate. Reagent 1: (C2H5O)2P(O)C(O)OC2H5Reagent 2: an aqueous solution of NaON. Reaction conditions: heating the reaction mixture to 50C, followed by keeping the reaction mixture at the boiling, cooling the reaction mixture to a temperature not lower than 17C separation of the target product and its recrystallization by cooling an aqueous solution of the crude product is 20C or cooling to 5C With subsequent sushi formed dodecahydrate of trinitroresorcinate.

The invention relates to a method of synthesis of foscarnet, i.e. uranyl trinitroresorcinate.

The known method of synthesis of phosphonoformate alkali metals, comprising a stage of mixing trialkylphosphates and aqueous alkali metal hydroxide at a temperature between the melting point of water and 40aboutWith optional maintaining the reaction mixture at this temperature for some time, and then heating the reaction mixture to boiling under reflux for complete saponification. The product is then emit through the contents of the reaction which is 80-86% and a purity of 99.9%, However, was found, the water content, which should be 36% in dry product in hexahydrate form, changes in the implementation of the process according to the described method.

The aim of the invention is to develop a method for the synthesis of uranyl trinitroresorcinate. This objective is achieved in accordance with the invention, which is characterized by the steps of adding sodium hydroxide to the water, heating the aqueous solution of sodium hydroxide to 50aboutWith, add to the specified solution triethylphosphite at 50aboutWith, heating the reaction mixture up to the boiling temperature under reflux for about 1 h, cooling the reaction mixture and filtering off the product.

According to one variant of the invention, the product is dissolved in water and then recrystallized by cooling the solution to about 20aboutWith getting the uranyl trinatriytsitrat. According to another variant of the invention, the product is dissolved in water and then recrystallized by cooling the solution to about 5aboutWith, deliver dodecahydrate of trinitroresorcinate, which is dried, receiving the uranyl trinitroresorcinate.

According to the invention, what about the 50aboutC. and Then added to a solution of triethylphosphine at 50aboutC. the Temperature of the reaction mixture raised to the boiling temperature under reflux, i.e., approximately 90-95aboutC, and the resulting ethanol is distilled off. After finding within a reasonable time at the boiling point under reflux, which should be approximately 1 h, the reaction mixture is cooled and the product filtered off.

Cooling to a temperature not lower than approximately 17aboutWith, preferably not lower than 20aboutC leads to the formation of uranyl trinitroresorcinate in the wet state. The water content is thus about 36% which is the water content of the dry product in pure form. Cooling to temperatures above 20aboutWith leads to reduced output. As a suitable upper limit, which still get adequate output, can be 25-30aboutC.

Cooling to about 5aboutWith or below leads to the formation of dodecahydrate of trinitroresorcinate. After drying of this compound in suitable conditions, the product in dodecahydrate the form is then transformed into hexahydrate form. If processlifetime.

The product obtained according to the invention, preferably recrystallized by dissolving it in water, heating the solution to obtain a clear solution which is then cooled down to nearly 20aboutWith to get the product in hexahydrate form, or up to about 5aboutWith to get the product in dodecahydrate form for further drying.

P R I m e R 1. 423 g (4.77 mol) of sodium hydroxide in the form of a concentrated liquid added to 400 ml of water. The solution is heated to approximately the 50aboutC and at this temperature add 167 g (0,795 mol) of triethylphosphite. The reaction mixture is then heated to approximately 90aboutWith and the resulting ethanol is distilled off. After about 1 h at 90-95aboutWith the reaction mixture is cooled to 20aboutWith, and the product is filtered. The output of the wet uranyl trinitroresorcinate is 248, Wet substance is recrystallized in 570 ml of water by heating to 90aboutIn order to obtain a clear solution and then cooled to about 20aboutC. After filtration and washing with 50 ml of water at 18-22aboutTo get 187 g (74% of theoretical yield) of uranyl trinitroresorcinate. This substance content is ATA trinitroresorcinate dissolved in 335 ml of water with heating to 90aboutWith obtaining a clear solution and then cooled to about 5aboutC. After filtration obtain 119 g of dodecahydrate of trinitroresorcinate. Drying the substance in suitable conditions, leads to the formation of uranyl trinitroresorcinate.

The METHOD of producing URANYL TRINITRORESORCINATE processing triethylphosphite aqueous solution of sodium hydroxide, heating the reaction mixture to boiling point, cooling the reaction mixture and separation of the target product with subsequent recrystallization from an aqueous solution, characterized in that the processing triethylphosphite lead at the 50oWith pre-heated up to this temperature with an aqueous solution of sodium hydroxide, cooling the reaction mixture is conducted to a temperature not lower than the 17oWith, preferably up to 20oWith, and recrystallization is carried out by cooling the aqueous solution of the crude product to the 20oWith and separating the resulting crystals or cooling of this solution to 5oWith subsequent drying of the resulting dodecahydrate of trinitroresorcinate to obtain uranyl trinitroresorcinate.

 

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