The method of obtaining 1,4,3,6-dianhydro-d-sorbitol dinitrate

 

(57) Abstract:

The invention relates to a technology for 1,4,3,6-dianhydro-D-sorbitol dinitrate, which is the substance of the medicinal product "nitrosorbid". The method of obtaining 1,4,3,6-dianhydro-D-sorbitol dinitrate is in the nitration 5.1-6.9 wt.D. nitric acid at a temperature of 0-17oWith 1 wt. D. 1,4,3,6-dianhydro-D-sorbitol dinitrate containing 0.5 to 9.5% of the water supplied to the nitration temperature 40-80oC. after completing the reaction mass is diluted with wash water to a content of nitric acid, 20-25%, nitrosorbid filtered from the spent acid and washed with water. The proposed solution will reduce the consumption of nitric acid, to improve the performance of the nitration process, reduce the amount of waste nitric acid used for regeneration. table 1.

The invention relates to a technology for 1,4,3,6-dianhydro-D-sorbitol dinitrate (nitrosorbid), which is the substance of a medicinal product under the name "nitrosorbid", which is used as a vasodilator to treat hypertension, angina and other cardiovascular diseases.

NITR is known laboratory method of nitration of sorbed sulfuric-nitric mixture (melange), the proposed UNIFI them. S. Ordzhonikidze ( P. M. Kochergin, R. M. Titkov. The medical industry of the USSR, 8, 18, 1959), which requires validation in an industrial environment. Its disadvantages are the complexity of the regeneration of the mixed waste acid and wash water compared with the regeneration of one of nitric acid.

Most noteworthy is the way nitration of sorbed nitric acid and allocation nitrosorbid by diluting the reaction mixture with water, which is implemented at a chemical plant in Krasnouralsk the Ekaterinburg region) and adopted for the prototype (Regulations for obtaining nitrosorbid in poltavtsom scale, UNIFI them. S. Ordzhonikidze, 1963).

In this way nitrosorbid obtained by adding a concentrated aqueous solution of 1 weight. including carbide (syrupy liquid that contains 80-90% of sorbed) to fuming nitric acid at a temperature of 18-20oC for 1 -1 h 20 min Nitric acid taken in the quantity of 7.75 weight.h. 1 century including carbide. Instead of nitric acid as nitrouse agent can be applied melange (mixture of nitric and sulphuric acids) in the same ratio. At the end of dosing an aqueous solution of sorbide the reaction mass is maintained at 16-20oC for 30 min, and longer in the form of white crystals. The resulting suspension nitrosorbid in dilute nitric acid, filtered, the filter cake washed with water until neutral and sent for recrystallization in ethanol. Waste nitric acid (15-18% concentration) and wash water (1-4% concentration) is passed to regeneration.

The disadvantages of the method are:

- high consumption of nitric acid in the nitration;

the low concentration of the spent nitric acid upon dilution of the reaction mixture with clean water;

the costs of regeneration of nitric acid after water leaching;

- reduced the productivity of the process.

The aim of the present invention is to reduce the consumption of nitric acid, increasing productivity, reducing costs for the regeneration of spent acid and wash water.

This goal is achieved by reducing additives water to carbide applied to the nitration, 0.5-9.5% and reduction of the nitric acid in the nitration with 7,75 wt.D. to 5.1-6.9 wt.D., replacement of pure water for dilution sour wash water, reducing the amount of spent acid used for regeneration.

Nitration of sorbed nitrogen Kim, stirrer, water (brine) bath for cooling, download 510-690 g of 98.5% nitric acid, cooled her from minus 2oTo + 12oAnd when the agitator from a heated dropping funnel dispense heated to 40-80oWith sorbed in the number of 100.5-109,5 g containing 0.5 to 9.5% of water, maintaining the temperature in the reaction mass 0-17oC. Upon completion of the dosage sorbed give exposure 30 min at 10-17oWith, and then the resulting reaction mass slowly with stirring 12-17oWith poured in 2-2,3 l wash "acidic" water from the previous water leaching. Suspension nitrosorbid diluted in up to 20-25% nitric acid, filtered, nitrosorbid portions washed with water, which is used for dilution, and nitrosorbid dried at a temperature of 50-60oWith and analyze the requirements of the Federal Assembly of 42-422-92. Waste nitric acid regenerate known methods. The content of the basic substance in carbide 98-99% define chromatographic, and when the content of the basic substance 95-97% sorbed again distilled under a residual pressure of 1-5 kPa and a temperature of 165-195oC.

The hallmark of this method is the reduction of water content in carbide impede the process of nitration and Spole to reduce the consumption of nitric acid, to increase the productivity of the process nitrile, reduce the amount of waste nitric acid for regeneration. Mobility "syrup" carbide for dosing with a reduced water content reached by raising its temperature with a water content of 0.5% to 75-80oWith due to its melting point, when the water content of 6-9,5% to 40-45oWith the expense of increasing the solubility and fluidity.

The results of the experiments presented in the table.

The method of obtaining 1,4,3,6-dianhydro-D-sorbitol dinitrate by nitration with nitric acid flooded 1,4,3,6-dianhydro-D-sorbitol, containing not less than 98% of the basic substance, and separating it from the reaction mixture by dilution with water, characterized in that the 5.1-6.9 wt. D. nitric acid is dosed 1 wt. D. with a temperature of 40-80oWith 1,4,3,6-dianhydro-D-sorbitol containing 0.5 to 9.5% of water, maintaining the temperature of the reaction mass 0-17oAnd for dilution of the reaction mixture to 20-25% concentration of nitric acid used water after washing, isolated from the reaction mass 1,4,3,6-dianhydro-D-sorbitol dinitrate.

 

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< / BR>
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