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Creatine phosphate sodium preparation method

A technology of sodium creatine phosphate and chlorophosphoric acid, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as high production costs, cumbersome post-processing, and harmfulness of barium. Achieve the effects of low production cost, simple post-processing, and pollution reduction

Active Publication Date: 2012-08-15
NANJING CHENGONG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purification of the final product of this process needs to pass through anion exchange resin and cation exchange resin, the post-treatment is cumbersome and the production cost is high
[0018] In summary, the shortcomings of the prior art for preparing sodium creatine phosphate can be summarized as follows: first, most methods use barium ions, and the barium salts that can be introduced in the product not only affect the purity of the product in the downstream purification process, but also As a heavy metal, barium is extremely harmful to the human body; secondly, the biological enzymatic production process requires complicated requirements, inconvenient operation, and high production costs; moreover, due to other defects, it is inevitable to enter the complex purification process

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0047] a) In the reaction flask equipped with sodium hydroxide absorption device, add phosphorus oxychloride POCl 3 (153.33g, 1.0mol), cool down in an ice-water bath to 0°C~5°C, slowly add deoxygenated water (36g, 2.0mol) dropwise, after the addition, control the temperature of the reaction solution at 5°C~10°C and stir for 2 hours. Airtight storage for later use;

[0048] b) In the reaction flask equipped with sodium hydroxide absorption device, add S-methylisothiourea (60.0g, 0.67mol), N,N-dimethylformamide DMF 600mL, stir well and add the above prepared Chlorophosphoric acid 1mol, control the temperature of the reaction solution at 35°C~40°C and stir for 5 hours, evaporate N,N-dimethylformamide under reduced pressure to obtain phosphorylated S-methylisothiourea (114g, 0.67mol). The intermediate of this step reaction does not need to be purified in full amount to continue to do it;

[0049] c) In the reaction flask equipped with a sodium hydroxide absorption device, add th...

Embodiment 2

[0052] a) In the reaction flask equipped with sodium hydroxide absorption device, add phosphorus oxychloride POCl 3 (153.33g, 1.0mol), cooled in an ice-water bath to 0°C~5°C, slowly added deoxygenated water (36g, 2.0mol) dropwise, after the addition, controlled the temperature of the reaction solution at 0°C~5°C and stirred for 3 hours. Airtight storage for later use;

[0053] b) Add S-methylisothiourea (45.0g, 0.50mol) and 450mL dimethyl sulfoxide into the reaction flask equipped with a sodium hydroxide absorption device, stir well and add 1mol of chlorophosphoric acid prepared above to control the reaction The solution was stirred at a temperature of 20°C to 30°C for 6 hours, and the dimethyl sulfoxide was distilled off under reduced pressure to obtain phosphorylated S-methylisothiourea (85.0 g, 0.5 mol). The intermediate of this step reaction does not need to be purified in full amount to continue to do it;

[0054] c) Add the phosphorylated S-methylisothiourea (85.0g, 0....

Embodiment 3

[0057] a) In the reaction flask equipped with sodium hydroxide absorption device, add phosphorus oxychloride POCl 3 (153.33g, 1.0 mol), cool down to 0°C~5°C in an ice-water bath, slowly add deoxygenated water (36 g, 2.0 mol) dropwise, after the addition, control the temperature of the reaction solution at 2°C~7°C and stir for 2.5 hours . Airtight storage for later use;

[0058] b) Add S-methylisothiourea (60.0g, 0.67mol) and 600mL of acetone to the reaction flask equipped with a sodium hydroxide absorption device, stir well and add 0.67mol of chlorophosphoric acid prepared above to control the temperature of the reaction solution Stir at 40°C~50°C for 2 hours, distill off the acetone under reduced pressure to obtain phosphorylated S-methylisothiourea (114g, 0.67mol). The intermediate of this step reaction does not need to be purified in full amount to continue to do it;

[0059] c) In the reaction flask equipped with a sodium hydroxide absorption device, add the phosphoryla...

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Abstract

The invention relates to a creatine phosphate sodium preparation method, which includes the following steps of a), subjecting phosphorus oxychloride and water to be reacted at the temperature ranging from 0 DEG C to 10 DEG C for 2-3 hours to generate chlorophosphate; b), subjecting S-methyl isothiourea sulfate and chlorophosphate to react in dipole non-proton solvent to generate phosphorylated S-methyl isothiourea; c), dissolving the phosphorylated S-methyl isothiourea by adding water to be reacted with sarcosine to generate phosphocreatine; and d), adding sodium hydroxide orsodium methylate to the phosphocreatine to adjust the pH (potential of hydrogen) value to be 8-9, adding absolute ethyl alcohol, crystallizing, filtering and drying in vacuum to obtain creatine phosphate sodium. Phosphate group is introduced by preparing active chlorophosphate by phosphorus oxychloride, so that usage of phosphorus oxychloride can be reduced greatly, and environment pollution is alleviated correspondingly. The creatine phosphate sodium preparation method is a barium-free process, has no requirement for introducing heavy metal, safe, simple in post-treatment, high in yield and low in production cost, and byproducts are gases.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical engineering, and relates to a preparation method of creatine phosphate sodium, in particular to a preparation method of creatine phosphate sodium which is a drug for the cardiovascular system. Background technique [0002] Sodium creatine phosphate was developed by Ouhui Pharmaceutical Factory. It was first launched in Italy in 1992 and has been launched in Russia, Poland, Argentina and other countries. In 1995, my country began to import this product with the trade name "Huxintong". In 2000, the State Food and Drug Administration approved the listing of "Neoton" (Neoton) of Italy's Alpha Wesman Pharmaceutical Company in China. Creatine Phosphate Sodium English name is Creatine PHospHate Sodium, chemical name is N-[imino (phosphine amino) methyl]-N-methylglycine disodium salt tetrahydrate, CAS: 922-32-7, molecular weight: 327.14 , the chemical structural formula is as follows: [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/22
Inventor 郭昭
Owner NANJING CHENGONG PHARM CO LTD
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