Manganese(ii) succinate tetrahydrate preparation method

FIELD: organic synthesis.

SUBSTANCE: invention concerns an improved method for synthesis of manganese(II) succinate tetrahydrate wherein manganese(II) carbonate is portionwise added to succinic acid aqueous solution at molar ratio 1:1:4.5, respectively, under continuous stirring and, while maintaining constant temperature 60-65°C, each subsequent portion being added after complete dissolution of preceding manganese carbonate portion, after which desired product is isolated via recrystallization. Method can be used under industrial-scale conditions.

EFFECT: improved purity of product and minimum reactants used.

3 dwg, 2 tbl, 5 ex

 

The invention relates to organic chemistry, in particular to a method of obtaining crystallohydrates salt of succinic acid with manganese from the substrate reaction - succinic acid (succinate) and reagent reaction - carbonate of manganese. This method allows you to get succinate manganese high purity, while in the reaction of transformation of the original substances eliminated the formation of incidental impurities. This gives the opportunity to use succinate manganese in pharmacology, medicine, veterinary medicine, food and chemical industries as drugs, biologically active additives and reagent in various syntheses.

Closest to the proposed invention is a method for succinate calcium by the interaction of calcium hydroxide or calcium carbonate with succinic acid in aqueous medium at 80°C for 3-6 hours when the reagent ratio 1:2-5 moles, respectively (U.S. Patent 3527798, CL. 260-537 SS 55/10). Disadvantages: to obtain consumes 2 mol of succinic acid, high temperature, which does not allow succinate manganese.

Known methods for producing succinate d-elements - of biologically active substances of complex action. The method consists in the action of sulfate corresponding d-metal mixture of succinic acid and the hydroxide is sodium in a ratio of 1:2 in moles at a temperature of 75-90° C for 20-30 minutes Method allows to obtain succinate d-elements of high purity (RF Patent No. 2174508, SS 51/41, 55/10). The disadvantage of this method is that to get succinate sulfate is used, which leads to the formation of the impurity stock solution as a salt of sodium sulfate, which ultimately leads to contamination of the target product.

You know getting succinate d-elements (iron, copper, zinc, manganese, cobalt) in the following way. To 0.1 M sodium of etexilate deviations add 200 ml of water, add 0.1 M succinic acid. The mixture is cooled to room temperature and add 0.1 M corresponding salts of the trace. Then the precipitate is filtered and dried (Patent RU 2092074, AK 1/16, Patent RU 2086149, AK 1/16). The disadvantage of this method is that the resulting reaction products are contaminated silicic acid and many of the reaction products do not dissolve in water.

Also known ways of getting succinate sodium with Acrylonitrile and sodium cyanide in the presence of palladium catalyst at 230°autoclave (Patent 57-20932, Japan, MKI SS 55/10, SS 55/10). The potassium succinate is produced by the action of carbon oxide (II) a mixture of carbonate and potassium acetate at 300-450°With (Patent 13012, Japan, CL SS 55/10). The disadvantage of this method is that it is quite difficult to perform data syntheses without soo the relevant equipment, and they are not acceptable to obtain succinate manganese.

The objective of the invention is to improve a method of producing manganese succinate of tetrahydrate with minimal use of reagents of the reaction, which does not contaminate the final product side by impurities in the process of transformation of the original substances.

The task of obtaining manganese succinate high purity with minimal use of reagents of the reaction is decided by the action of 1 mole of manganese carbonate to 1 mole of succinic acid dissolved in 4.5 moles of distilled water at a temperature of 60-65°C.

The proposed method is as follows.

In chemical glass beaker dissolve 0.1 mol (11.8 g) of succinic acid in 4.5 moles of distilled water at a temperature of 60-65°C. After complete dissolution of succinic acid to the solution in small portions at 3-4 g add 0.1 mol (11.5g) reagent reaction - carbonate of manganese. Each new portion of carbonate of manganese should be added after dissolved the previous and will cease to stand out bubbles of CO2. You must constantly stir the solution with a glass rod. The temperature of the mother liquor is maintained at the level of 60-65°C, until complete dissolution of carbonate of manganese. After completion of the synthesis of the glass covering the Ute filter paper, put in an ice bath and left overnight in the refrigerator. After days in the sediment fall pink crystals succinate manganese. Then the mother liquor was filtered to separate the crystals. The obtained crystals of manganese succinate is subjected to recrystallization. After recrystallization of the salt falls in the form of fine crystalline masses of light pink color, which is separated from the mother liquor by filtration on a Buchner funnel connected to a suction flask, and carefully squeezed from the mother liquor with a glass rod. The obtained crystalline salt is dried in air or in a thermostat at a temperature not exceeding 50°C.

Structure of manganese succinate established using x-ray analysis on a CAD4 diffractometer Enraf-Nonius (figure 1, figure 2, figure 3, table 1). Gross formula C4H12MnO8. Mass fraction of manganese 22,62% (table 2).

Thus, this method allows you to get succinate manganese high purity, while in the reaction of transformation of the original substances eliminated the formation of incidental impurities. The yield of the target product is 90-94%. (2) It enables you to use succinate manganese in pharmacology, medicine, veterinary medicine, food and chemical industries as drugs, biologically active EXT the Cai and reagent in various syntheses.

Examples of specific performance synthesis for the preparation of manganese succinate

Example 1. In pure chemical glass beaker dissolve 11.8 g of succinic acid in 81 ml of distilled water, pH 1.0 to 1.5. To this solution was added to 11.5 g of manganese carbonate, simultaneously, while stirring with a glass rod. When this happens bubbling CO2but is not the complete dissolution of carbonate of manganese. the pH of the solution is 2.3 to 3.5. In the result, almost all the amount of manganese carbonate settles to the bottom in an unmodified state. The synthesis does not occur.

Example 2. Synthesis start to spend on the above described example 1. But after dissolving succinic acid solution is heated to 60-65°C. then simultaneously added to 11.5 g of manganese carbonate while stirring with a glass rod. If the pH of the solution is 4.2 and 5.6. After cease to stand out bubbles of CO2the glass of solution is served filter paper and leave at room temperature. Thus, there is a deposition of larger amounts of manganese carbonate, the surface of which there is loss of single crystals light brown color. Not completed the equivalent synthesis. A large part of reagent - carbonate of manganese did not react with the substrate reaction - succinic acid is.

Example 3. The beginning of the synthesis is the same as in example 2. In 60-65°With a solution of succinic acid portions add carbonate of manganese from the total number of 11.5 g Each subsequent portion of the manganese carbonate added after the allocation of gas bubbles CO2and partial dissolution of the reagent. The temperature of the solution is statically not supported, that is gradually reduced. After adding the last portion of the manganese carbonate glass obtained substance is covered with filter paper and placed in an ice bath. By the end of the day a significant part of the reagent - carbonate of manganese is deposited on the bottom of the glass on its surface a thin film rolled crystals light brown color. If you interfere with a glass rod the mother liquor, destroying the crystals, then after a day the amount of precipitated crystals increases, but the solution remains a significant amount of undissolved carbonate of manganese. The mother liquor from the crystals filtered off. The obtained crystals clear of carbonate of manganese and other impurities by recrystallization. Practical output succinate manganese has low efficiency.

Example 4. The synthesis starts the same way as in example 3. After complete dissolution of succinic acid to the solution in small portions add the reagent reaction - carbonate of manganese. Each but the second portion of carbonate of manganese should be added after as will dissolve the previous and will cease to stand out bubbles of CO2, while stirring the solution with a glass rod. If the pH of the solution is gradually shifted to neutral reaction, and after the dissolution of the last portion of the reagent pH equal to 7.0 to 7.2. This requires 11.5g reagent reaction of manganese carbonate. The temperature of the mother liquor is maintained at the level of 60-75°to dissolve the carbonate of manganese. After synthesis, the beaker is covered with a filter paper, put in an ice bath and left overnight in the refrigerator. After days in the sediment fall light pink crystals of manganese succinate. Then the mother liquor is filtered to separate the crystals. The obtained crystals of manganese succinate is subjected to recrystallization. After recrystallization succinate manganese is precipitated in the form of a crystalline mass of white with a pink tinge, which is separated from the mother liquor by filtration on a Buchner funnel connected to a suction flask, and thoroughly wrung out from the mother liquor with a glass rod. The obtained crystalline drug is dried in air or thermostat at a temperature not exceeding 50°C.

Example 5. The synthesis begins to example 3. After adding the first portion of the reagent to the of rbonate manganese solution is brought up to 80-100° C. the Temperature of the solution is maintained at the level 80-100°until then, until completely dissolved the entire portion of carbonate of manganese. After the dissolution of the last portion of the manganese carbonate glass reaction product is served filter paper and placed in an ice bath. Thus, there is a loss of black, insoluble in water, sediment and small amounts of brown crystals of manganese succinate.

Table 1

Basic crystallographic characteristics of manganese succinate
IndexThe value of the index
Gross formulaWith4H12MnO8
M243,08
A, K293
Crystal systemTriclinic
Space groupR-1

Table 2

Quality indicators manganese succinate
IndicatorsThe value of the index
1 appearanceCrystalline powder light pink color
2 TasteSour bitter
3 Smell Odourless
4 Mass fraction of manganese, %22,6
5. Melting point, °103
6. SolubilityIn water soluble in alcohol, benzene insoluble
Fractiously output %90-94%
8. The molar ratio maturity (ελ), 0.1 M solution of females. manganese35,72
9. The wavelength at which the maximum spectral absorption of 0.1 M solution of females. manganese (λmax), nm226

A method of producing manganese succinate tetrahydrate, characterized in that as a reagent reaction is used carbonate manganese (II), which portions are added to aqueous solution of succinic acid in the ratio 1:1:4.5 moles with constant stirring and continuously maintaining the temperature of 60-65°With each subsequent batch is added only after the complete dissolution of the previous portion of carbonate of manganese, followed by separation of the target product by recrystallization.



 

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