Microwave synthesis method of taurine magnesium salt
The reaction of water, taurine and magnesium compounds by microwave synthesis method has solved the problems of low salt yield and incomplete reaction in the existing magnesium taurine salt preparation method, and achieved an efficient, safe and environmentally friendly preparation process, with wide application prospects.
Patent Information
- Application Number
- CN202510036680.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-09
- Publication Date
- 2025-05-02
AI Technical Summary
The existing preparation methods for magnesium taurate salt have problems such as low salt formation rate, incomplete reaction, and safety hazards in the process.
Using microwave synthesis method, water, taurine and magnesium compounds are reacted under microwave action, and then magnesium taurine salt is obtained by rotary vaporization, concentration, crystallization and drying steps.
It improves the salt formation rate of taurine, shortens the reaction time, improves heat transfer efficiency, is simple and stable in the process, is environmentally friendly and has no by-products, and has broad application prospects.
Smart Images
Figure CN119912367A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of medical technology, and in particular to a microwave synthesis method of taurine magnesium salt. Background Art
[0002] Magnesium is one of the essential metal elements in the human body. Magnesium participates in multiple pathways of metabolism and protein synthesis in the human body, and can activate multiple enzymes in the body; various types of magnesium salts are widely used in clinical practice. Taurine is one of the common sulfur-containing amino acids in humans and animals, and taurine is widely distributed in various tissues and organs in the body. Magnesium salt of taurine has anti-hypertensive, anti-arrhythmic, anti-preeclampsia and eclampsia effects, and can be used as a feasible new therapeutic drug, food additive and metal element supplement. At present, there have been reports on clinical studies of magnesium taurine, and magnesium taurine capsules have been launched in the UK. Magnesium taurine has good salt solubility, good stability, and easy absorption, so it has broad application prospects.
[0003] There are few literature reports on the preparation methods of taurine magnesium salt, and the traditional preparation methods have problems such as low salt formation rate, incomplete reaction, and potential safety hazards in the process. Therefore, it is necessary to propose a new efficient, safe and environmentally friendly method for preparing taurine magnesium salt to solve some of the above problems. Summary of the invention
[0004] The technical problem to be solved by the present invention is to provide a microwave synthesis method of taurine magnesium salt in view of the deficiencies in the above-mentioned prior art.
[0005] In order to solve the above technical problems, the technical solution adopted by the present invention is: a microwave synthesis method of taurine magnesium salt, comprising the following steps:
[0006] S1, mixing water, taurine and a magnesium compound, and reacting them under the action of microwaves;
[0007] S2. After the reaction is completed, the product obtained in step S1 is subjected to rotary evaporation and concentration, and then a single post-treatment solvent is added to crystallize, filtered and dried to obtain taurine magnesium salt.
[0008] Preferably, the magnesium compound in step S1 includes, but is not limited to, magnesium hydroxide, light magnesium carbonate, heavy magnesium carbonate, basic magnesium carbonate, etc., and magnesium hydroxide is most preferred.
[0009] Preferably, the molar ratio of the magnesium compound to taurine is 0.9:2 to 1.1:2, for example, 0.9:2, 1.0:2, 1.1:2 or any value between them, and most preferably 1.0:2.
[0010] Preferably, the volume of water used is 5 to 20 times the weight of taurine, measured in mL by volume and g by weight, for example, 5, 10, 15, 20 times or any value therebetween, and most preferably 10 times.
[0011] Preferably, the microwave power applied in step S1 is 100-2000W, corresponding to a feed amount of 5g or 50g, and most preferably 300W or 2000W.
[0012] Preferably, the frequency of the microwave applied in step S1 is 300 MHz to 300 GHz, most preferably 2450 MHz.
[0013] Preferably, the reaction temperature in step S1 is 60-100°C, for example, 60°C, 70°C, 80°C, 90°C, 100°C or any value therebetween, and most preferably 100°C.
[0014] Preferably, the reaction time in S1 is 0.5-2.0 h; for example, it can be 0.5, 1.0, 1.5, 2.0 h or any value therebetween, and most preferably is 1.0 h.
[0015] Preferably, the single post-treatment solvent in step S2 is selected from at least one of ethanol, methanol, isopropanol, acetone and tetrahydrofuran, and most preferably is ethanol.
[0016] Preferably, the volume of the single post-treatment solvent in step S2 is 3 to 10 times the weight of taurine, measured in mL by volume and g by weight, for example, 3, 5, 7, 10 times or any value therebetween, most preferably 5 times.
[0017] Preferably, the microwave synthesis method of taurine magnesium salt comprises the following steps:
[0018] S1, adding water, taurine and magnesium compound into a microwave reactor and mixing, turning on the microwave reactor, setting the microwave reactor power to 100-2000W, the frequency to 300MHz-300GHz, and reacting at 60-100°C for 0.5-2.0h;
[0019] S2. After the reaction is completed, the product obtained in step S1 is transferred to a rotary evaporator, concentrated at 50-70°C, and then a single post-treatment solvent is added. The product is stirred and crystallized at room temperature for 1-4 hours. After filtering, the solid product is rinsed with a single post-treatment solvent and then dried to obtain taurine magnesium salt.
[0020] The beneficial effects of the present invention are:
[0021] The present invention provides a microwave synthesis method of taurine magnesium salt, which uses taurine, which is cheap and easily available in large-scale industrial production, as a raw material, and a magnesium compound such as magnesium hydroxide or magnesium carbonate in water for microwave reaction, so as to synthesize taurine magnesium salt simply and efficiently. The microwave synthesis method solves the problem of slow heterogeneous reaction speed caused by the insolubility of magnesium hydroxide and magnesium carbonate in water at the microscopic level, so that magnesium hydroxide and taurine can be dissolved in the water phase after salt formation faster, thereby improving the salt formation rate of taurine; the higher thermal effect of microwaves also better improves the heat transfer efficiency inside the reaction system, greatly accelerating the reaction speed. The process method of the present invention is green and environmentally friendly, and does not produce environmentally harmful by-products; and the process is simple and stable, the reaction speed is fast, the reaction conditions are relatively mild, the raw materials are all commercially available, cheap and easy to obtain, the yield is high, and it has broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 This is the NMR spectrum of the finished taurine magnesium salt prepared in Example 1. DETAILED DESCRIPTION
[0023] The present invention is further described in detail below in conjunction with embodiments so that those skilled in the art can implement the invention with reference to the description.
[0024] It should be understood that the terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.
[0025] The test methods used in the following examples are conventional methods unless otherwise specified. The materials and reagents used in the following examples are all commercially available unless otherwise specified. In the following examples, if no specific conditions are specified, the experiments were carried out under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used, if the manufacturer is not specified, are all conventional products that can be purchased commercially.
[0026] Example 1
[0027] A microwave synthesis method for taurine magnesium salt, the synthesis route and main reaction conditions are as follows:
[0028]
[0029] The specific steps are:
[0030] S1. Add 50 mL of water to a microwave reactor, and then add taurine (5.00 g, 40.0 mmol) and magnesium hydroxide (1.17 g, 20.0 mmol) in sequence to disperse into a uniform white suspension. Turn on the microwave reactor and set the microwave reactor power to 300 W, frequency to 2450 MHz, reaction temperature to 100 ° C, and reaction time to 1.0 h.
[0031] S2. After the reaction is completed, the obtained colorless clear liquid is transferred to a rotary evaporator, the temperature is raised to 55°C, and the liquid is concentrated under reduced pressure until there is no droplet. 25 mL of anhydrous ethanol is added to precipitate a white solid, and the solid is stirred and crystallized at room temperature for 2 h; filtered, the wet product is rinsed with 5 mL of ethanol twice, and dried at 70°C to obtain 5.37 g of taurine magnesium salt as a white powder with a yield of 98.5%.
[0032] After testing, the moisture content of the sample was 0.45% (the detection method was based on the water determination method (Karl Fischer method) in Part IV of the 2020 edition of the Chinese Pharmacopoeia), and the theoretical value of the moisture content of taurine magnesium salt was 0%; the magnesium content of the sample was 8.67% (the detection method was based on the inductively coupled plasma mass spectrometry method in Part IV of the 2020 edition of the Chinese Pharmacopoeia), and the theoretical value of the magnesium content of taurine magnesium salt was 8.91%; it can be determined that the obtained sample is indeed taurine magnesium salt (without crystal water).
[0033] The NMR spectrum of the taurine magnesium salt product prepared in this example is as follows Figure 1 As shown, the NMR data are as follows:
[0034] 1 H NMR (400MHz, D2O): δ = 3.12 (m, 2H), 3.04 (m, 2H).
[0035] Example 2
[0036] A microwave synthesis method for taurine magnesium salt, the synthesis route and main reaction conditions are as follows:
[0037]
[0038] The specific steps are:
[0039] S1. Add 50 mL of water to a microwave reactor, and then add taurine (5.00 g, 40.0 mmol) and light magnesium carbonate (1.69 g, 20.0 mmol) in sequence to disperse into a uniform white suspension. Turn on the microwave reactor and set the microwave reactor power to 300 W, frequency to 2450 MHz, reaction temperature to 100 ° C, and reaction time to 1.0 h.
[0040] S2. After the reaction is completed, the obtained colorless clear liquid is transferred to a rotary evaporator, the temperature is raised to 55°C, and the liquid is concentrated under reduced pressure until there is no droplet. 25 mL of anhydrous ethanol is added to precipitate a white solid, and the solid is stirred and crystallized at room temperature for 2 h; filtered, the wet product is rinsed with 5 mL of ethanol twice, and dried at 70°C to obtain 5.29 g of taurine magnesium salt as a white powder with a yield of 97.1%.
[0041] Example 3
[0042] A microwave synthesis method for taurine magnesium salt, the synthesis route and main reaction conditions are as follows:
[0043]
[0044] The specific steps are:
[0045] S1. Add 500 mL of water to a microwave reactor, and then add taurine (50.00 g, 400.0 mmol) and magnesium hydroxide (11.7 g, 200.0 mmol) in sequence to disperse into a uniform white suspension. Turn on the microwave reactor and set the microwave reactor power to 2000 W, frequency to 2450 MHz, reaction temperature to 100 ° C, and reaction time to 1.0 h.
[0046] S2. After the reaction is completed, the obtained colorless clear liquid is transferred to a rotary evaporator, the temperature is raised to 55°C, and the liquid is concentrated under reduced pressure until there is no droplet. 250 mL of anhydrous ethanol is added to precipitate a white solid, and the solid is stirred and crystallized at room temperature for 2 h; filtered, the wet product is rinsed with 50 mL of ethanol twice, and dried at 70°C to obtain 52.4 g of taurine magnesium salt as a finished product, which is a white powder with a yield of 96.1%.
[0047] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to specific details.
Claims
1. A microwave synthesis method for taurine magnesium salt, characterized in that: The following steps are involved: S1, mixing water, taurine and a magnesium compound, and reacting them under the action of microwaves; S2. After the reaction is completed, the product obtained in step S1 is subjected to rotary evaporation and concentration, and then a single post-treatment solvent is added to crystallize, filtered and dried to obtain taurine magnesium salt.
2. The microwave synthesis method of taurine magnesium salt according to claim 1, characterized in that: The magnesium compound in step S1 is at least one selected from magnesium hydroxide, light magnesium carbonate, heavy magnesium carbonate, and basic magnesium carbonate.
3. The microwave synthesis method of taurine magnesium salt according to claim 2, characterized in that: The molar ratio of the magnesium compound to taurine is 0.9:2 to 1.1:
2.
4. The microwave synthesis method of taurine magnesium salt according to claim 1, characterized in that: The volume of water used in step S1 is 5 to 20 times the weight of taurine, with the volume unit being mL and the weight unit being g.
5. The microwave synthesis method of taurine magnesium salt according to claim 1, characterized in that: The microwave power applied in step S1 is 100-2000W; 6. The microwave synthesis method of taurine magnesium salt according to claim 5, characterized in that: The frequency of the microwave applied in step S1 is 300 MHz to 300 GHz.
7. The microwave synthesis method of taurine magnesium salt according to claim 6, characterized in that: The reaction temperature in step S1 is 60-100°C, and the reaction time is 0.5-2.0h; 8. The microwave synthesis method of taurine magnesium salt according to claim 1, characterized in that: The single post-treatment solvent in step S2 is selected from at least one of ethanol, methanol, isopropanol, acetone and tetrahydrofuran.
9. The microwave synthesis method of taurine magnesium salt according to claim 8, characterized in that: The volume of the single post-treatment solvent in step S2 is 3 to 10 times the weight of taurine, measured in mL by volume and g by weight.
10. The microwave synthesis method of taurine magnesium salt according to claim 1, characterized in that: The following steps are involved: S1, adding water, taurine and magnesium compound into a microwave reactor and mixing, turning on the microwave reactor, setting the microwave reactor power to 100-2000W, the frequency to 300MHz-300GHz, and reacting at 60-100°C for 0.5-2.0h; S2. After the reaction is completed, the product obtained in step S1 is transferred to a rotary evaporator, concentrated at 50-70°C, and then a single post-treatment solvent is added. The product is stirred and crystallized at room temperature for 1-4 hours. After filtering, the solid product is rinsed with a single post-treatment solvent and then dried to obtain taurine magnesium salt.