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Synthesis of phosphocreatine disodium salt

A technology of creatine phosphate disodium salt and disodium creatine phosphate, which is applied in the field of high-energy compounds, can solve the problems of unrecoverable raw materials, high cost, and low yield, and achieve more product purification times, increased costs, and increased purification times Effect

Inactive Publication Date: 2012-01-11
上海慈瑞医药科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The barium salt process mostly uses creatine as raw material to synthesize creatine phosphate, such as the method reported in the Journal of Harbin Institute of Technology (2004, 9 volumes 4, 124 pages-126 pages), the method yield is low, the raw materials cannot be recycled, and the waste is relatively high. Big
Barium-free technology such as US3036087 uses dibenzyl phosphite and methyl isothiourea as raw materials to synthesize creatine phosphate sodium through multi-step reactions. The synthesis route of this method is too long, and toxic reagents such as mercury oxide are used in the reaction, so in In actual production, the safety protection requirements are high, and the cost is correspondingly high

Method used

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  • Synthesis of phosphocreatine disodium salt
  • Synthesis of phosphocreatine disodium salt
  • Synthesis of phosphocreatine disodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of synthetic method of creatine phosphate disodium salt is:

[0022] The first step. dissolving disodium creatinine phosphate in 2 times the weight of water, decolorizing with 5% of the weight of activated carbon in an ice-water bath, filtering, adding 4 times the weight of ethanol to the filtrate, and suctioning to obtain disodium creatinine phosphate products;

[0023] The second step. Dissolve the refined product of disodium creatinine phosphate prepared in the first step in 2 times the weight of water, add 10% times the weight of activated carbon, stir in an ice-water bath for 1 hour, filter, and add hydrogen to the filtrate Adjust the pH of the solution to 13 with sodium oxide, stir at 80°C for 0.1 hour, then adjust the pH to 7 with hydrochloric acid in an ice-water bath, decolorize with 20% of the weight of activated carbon at room temperature, filter, add 6 times the weight of ethanol to the filtrate, and continue stirring at room temperature for 12 hours....

Embodiment 2

[0028] A kind of synthetic method of creatine phosphate disodium salt is:

[0029] The first step. dissolving disodium creatinine phosphate in 5 times the weight of water, decolorizing with 20% of the weight of activated carbon in an ice-water bath, filtering, adding 40 times the weight of ethanol to the filtrate, and suctioning to obtain disodium creatinine phosphate products;

[0030] The second step. Dissolve the refined product of disodium creatinine phosphate prepared in the first step in 6 times the weight of water, add 20% times the weight of activated carbon, stir in an ice-water bath for 1 hour, filter, and add hydrogen to the filtrate Adjust the pH of the solution to 13 with sodium oxide, stir at 50°C for 18 hours, then adjust the pH to 8.5 with hydrochloric acid in an ice-water bath, decolorize with 10% of the weight of activated carbon at room temperature, filter, add 46 times the weight of ethanol to the filtrate, and continue stirring at room temperature for 12 ...

Embodiment 3

[0035] A kind of synthetic method of creatine phosphate disodium salt is:

[0036] The first step. dissolving disodium creatinine phosphate in 8 times the weight of water, decolorizing with 10% of the weight of active carbon in an ice-water bath, filtering, adding 80 times the weight of ethanol to the filtrate, and suctioning to obtain disodium creatinine phosphate products;

[0037] The second step. Dissolve the refined product of disodium creatinine phosphate obtained in the first step in 10 times the weight of water, add 5% times the weight of activated carbon, stir in an ice-water bath for 1 hour, filter, and add hydrogen to the filtrate Adjust the pH of the solution to 14 with sodium oxide, stir at 20°C for 36 hours, then adjust the pH to 10 with hydrochloric acid in an ice-water bath, decolorize with 5% of the weight of activated carbon at room temperature, filter, add 100 times the weight of ethanol to the filtrate, and continue stirring at room temperature for 12 hours...

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Abstract

The invention relates to a synthetic method of disodium creatine phosphate, which is characterized in that a barium-free salt operation method is adopted. In the method, disodium creatinine phosphate is dissolved in water, activated carbon is used in ice-water bath for decolorizing, the filtering is carried out, ethanol is added to filtering liquid, and after the air pump filtration, refined products of the disodium creatinine phosphate are obtained; the refined products of the disodium creatinine phosphate are dissolved in water, the activated carbon is added, and then the refined products are stirred and filtered in the ice-water bath, sodium hydroxide regulating solution with pH value of 13-14 is added to the filtrate and stirred, hydrochloric acid is used in the ice-water bath to regulate the pH value to 7-10, the activated carbon is used for decolorizing at the room temperature, the filtering is carried out, ethanol is added to the filtrate and stirred continuously, and the disodium creatine phosphate is obtained after the air pump filtration; the obtained disodium creatine phosphate is dissolved in water, activated carbon is added and stirred, the filtering is carried out, ethanol is added to the filtrate and stirred continuously, and the refined products of the disodium creatine phosphate are obtained after the air pump filtration. The synthetic method of the invention has the advantage of removing impurities produced during the preparing process of the disodium creatine phosphate to the utmost extent.

Description

technical field [0001] The invention relates to a method for synthesizing creatine phosphate disodium salt, in particular to a cardioprotective agent used in medical clinical cardiology and clinical surgery, and belongs to the technical field of high-energy compounds. Background technique [0002] Phosphocreatine (CP) is a high-energy compound containing high-energy phosphate bonds. It exists in large quantities in animal muscle cells. It is not only an important energy source for short-term, high-intensity sports, but also an important source of energy for the human body to start, accelerate, and adapt to rapid changes in environmental conditions. emergency energy. Since exogenous phosphocreatine is not listed as a stimulant, it has been widely used in sports in recent years. Creatine phosphate also has a series of physiological and biochemical functions, such as protecting skeletal muscle and cardiac muscle from intracellular damage caused by high-intensity training and c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/22A61P9/10
Inventor 金幸汤磊王立峰田雪飞
Owner 上海慈瑞医药科技股份有限公司
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