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Synthesis method of creatinol phosphate

A technique of myo-inositol phosphate and a synthesis method, which is applied in the field of organic synthesis, can solve problems such as increased equipment corrosion, acetic acid has a strong volatile odor, and difficulty in crystallization and separation, and achieves easy purification and recovery, low drying temperature, and increased yield and the effect of purity

Inactive Publication Date: 2017-11-24
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process also has difficulties in crystallization and separation, and acetic acid has a strong volatile odor, which increases the synthesis cost and harmful substances in the wastewater, and also increases the corrosiveness to equipment.

Method used

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  • Synthesis method of creatinol phosphate
  • Synthesis method of creatinol phosphate
  • Synthesis method of creatinol phosphate

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preparation example Construction

[0050] In view of this, in a specific embodiment of the present invention, a kind of synthetic method of inositol phosphate is provided, comprising steps as follows:

[0051] (1) Add lime nitrogen to the mixed solution of ethanol and water under a carbon dioxide atmosphere, continuously feed carbon dioxide to make the pH of the reaction solution to 7.5 to 8.5, and filter to obtain an ethanol solution of cyanamide;

[0052] (2) adding concentrated phosphoric acid to the ethanol and 2-(methylamino) ethanol solution to adjust the pH to 5-7, and adding dropwise the ethanol solution of cyanamide in the step (1) therein under the temperature condition of 50-70°C, The white myo-inositol phosphate was precipitated from the reaction, and myo-inositol phosphate was purified.

[0053] Wherein, the mass ratio of ethanol, lime nitrogen and water in step (1) (10-20): (3-5): (1-2), preferably 15:4:1; the pH of the reaction solution is 8; By adopting the above ratio, sufficient moisture can ...

Embodiment 1

[0070] (1) Add 300g of 95% ethanol and 25g of distilled water to a 1L reaction kettle with a mechanical stirrer, and then pass in carbon dioxide, add 80g of lime nitrogen to the reaction solution under stirring, and continue to pass in after the addition of lime nitrogen is completed Carbon dioxide to pH=8, stop the reaction, filter to obtain 256g of ethanol solution of cyanamide. During the whole reaction process, the reaction temperature is controlled below 50°C through a circulating water bath;

[0071] (2) In the reactor with mechanical stirrer, add 128g 95% ethanol and 32g 2-(methylamino) ethanol, add 52g 85% phosphoric acid to adjust pH to be 6, step (1) solution is dripped under the condition of 60 ℃ Added to the reaction system, directly reacted to obtain white inositol phosphate precipitate. Filter, wash with absolute ethanol, and vacuum-dry myo-inositol phosphate 68g (based on 2-(methylamino)ethanol, the yield is 74%).

[0072] Depend on figure 1 with figure 2 I...

Embodiment 2

[0074] (1) Add 320g of 95% ethanol, 20g of distilled water, and then carbon dioxide into a 1L reaction kettle with a mechanical stirrer, and add 96g of lime nitrogen into the reaction solution under stirring, and continue to feed the lime nitrogen after adding carbon dioxide to pH=8, stop the reaction, and filter to obtain 258 g of ethanol solution of cyanamide. During the whole reaction process, the reaction temperature is controlled below 50°C through a circulating water bath;

[0075] (2) In the reactor with mechanical stirrer, add 128g 95% ethanol and 32g 2-(methylamino) ethanol, add 52g 85% phosphoric acid to adjust pH to be 6, step (1) solution is dripped under the condition of 60 ℃ Added to the reaction system, directly reacted to obtain white inositol phosphate precipitate. Filter, wash with absolute ethanol, and vacuum-dry inositol phosphate 69g (calculated as 2-(methylamino)ethanol, the yield is 75%).

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Abstract

The invention discloses a synthesis method of creatinol phosphate. The synthesis method comprises the following steps: (1) adding lime nitrogen into mixed solution of ethanol and water under the carbon dioxide atmosphere, continuously guiding carbon dioxide into the mixture to adjust the pH value of reaction solution to 7.5-8.5, and filtering, so as to obtain cyanamide ethanol solution; and (2) adding strong phosphoric acid into ethanol solution and 2-(methylamino) ethanol solution to adjust the pH value to 5-7, dropping the cyanamide ethanol solution in Step (1) into the mixture at the temperature of 50-70 DEG C for reaction to obtain white creatinol phosphate precipitation, and purifying, so as to obtain the creatinol phosphate. In the synthesis method, ethanol is directly taken as a solvent, and a reaction of the ethanol solution containing a small amount of water and lime nitrogen is performed, so that the difficulty in crystallization and separation of a product caused by existence of the water can be effectively avoided. The method is low in cost of the raw materials, simple in processes, easy in industrial production, high in product purity and yield and small in the discharge amount of waste water, and therefore, the method conforms to the environment-friendly production concept.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for synthesizing inositol phosphate. Background technique [0002] Inositol phosphate is an important precursor for the synthesis of inositol phosphate. Myo-inositol phosphate converts ADP into ATP in the human body, so that ATP can be regenerated rapidly during intense activities to preserve muscle energy. Therefore, it is a high-efficiency sports food additive, which can quickly replenish energy and relieve muscle fatigue. The structure of myo-inositol contains a hydroxyl group. Compared with creatine containing a carboxyl group, it is less likely to undergo a cyclization reaction to generate creatinine. Therefore, myo-inositol can be phosphorylated to generate an energy substance like creatine. In addition, myo-inositol phosphate is very soluble in water and can be used as an additive for functional drinks to be directly consumed by the human body. With the rapid d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/08C07C277/08C01C3/16
CPCC07C277/08C01C3/16C07C279/08
Inventor 陈红余李平李璐秦坤
Owner TAISHAN MEDICAL UNIV
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