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Preparation method of creatinol phosphate

A technology of inositol phosphate and inositol phosphate, applied in the field of preparation of inositol phosphate, can solve problems such as lack of solutions, and achieve the effects of easy biochemical treatment, lowering reaction temperature and improving reaction efficiency

Active Publication Date: 2017-12-08
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] In summary, there are various problems in the preparation method of inositol phosphate in the prior art, and there is still a lack of effective solutions

Method used

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  • Preparation method of creatinol phosphate
  • Preparation method of creatinol phosphate
  • Preparation method of creatinol phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Add 150g ethyl acetate, 20g myo-inositol phosphate, p-toluenesulfonic acid 0.2g, dicyclohexylcarbodiimide (DCC) 10g successively in the 500mL flask of belt reflux device, under stirring state, reaction temperature is 90 ℃, reflux reaction for 3 hours, distill off 120 g of ethyl acetate under reduced pressure, and obtain a white solid after cooling and filtering. Add the solid to 100 g of distilled water, heat to 60° C. and filter while hot, cool to room temperature, filter and dry to obtain 17 g of white inositol phosphate, and the yield is 93% based on inositol phosphate.

[0047] Depend on figure 1 and figure 2 It can be seen that the product prepared by the present invention is inositol phosphate.

[0048] image 3 It is the high-efficiency liquid chromatogram of the synthetic product of embodiment 1, and table 1 is the analytical result table. Depend on image 3 As can be seen from Table 1, the purity of the prepared inositol phosphate is higher than 99%.

[...

Embodiment 2

[0052]Add 150g ethyl acetate, 20g myo-inositol phosphate, p-toluenesulfonic acid 0.2g, dicyclohexylcarbodiimide (DCC) 20g successively in a 500mL flask with a reflux device, and under stirring, the reaction temperature is 87 ℃, reflux reaction for 3 hours, distilled off 122 g of ethyl acetate under reduced pressure, cooled and filtered to obtain a white solid. The solid was added to 100g of distilled water, heated to 60°C and filtered while hot, cooled to room temperature, filtered and dried to obtain 16.8g of white inositol phosphate, and the yield in terms of inositol phosphate was 92%; the prepared inositol phosphate had a purity higher than 99%.

Embodiment 3

[0054] Add 100g of ethyl acetate, 20g of myo-inositol phosphate, 0.1g of p-toluenesulfonic acid, and 10g of dicyclohexylcarbodiimide (DCC) successively in a 500mL flask with a reflux device. Under stirring, the reaction temperature is 88 °C, reflux reaction for 3 hours, distill off 114 g of ethyl acetate under reduced pressure, cool and filter to obtain a white solid. Add the solid to 100 g of distilled water, heat to 60°C and filter while it is hot, cool to room temperature, filter and dry to obtain 15 g of white inositol phosphate, and the yield is 82% in terms of inositol phosphate; the purity of the prepared inositol phosphate is higher than 97% .

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Abstract

The invention discloses a preparation method of creatinol phosphate. The method comprises the following steps: uniformly mixing ethyl acetate, creatinol phosphate, p-toluenesulfonic acid and dicyclohexylcarbodiimide; heating and carrying out reflux reaction to obtain a creatinol phosphate crystal. As a catalyst, p-toluenesulfonic acid plays an effect of catalyzing creatinol and phosphoric acid in the creatinol phosphate to form ester. By using dicyclohexylcarbodiimide (DCC) as a dehydrating agent, water generated by performing esterification reaction is removed, so that the whole reaction is carried out completely, and the reaction yield is improved. Meanwhile, the ethyl acetate reaction solvent can be recycled, by-products and impurity parts produced in the reaction process are remained in ethyl acetate mother liquid, and the remaining DCC absorbs the water to produce 1,3-dicyclohexylurea (DCU); moreover, the DCU substance is insoluble in water, so that separation and purification are easily carried out in a recrystallization process, and the purity of the product is effectively ensured.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of inositol phosphate. Background technique [0002] Phosphoinositide is a new type of sports health care product additive. It is a high-efficiency sports supplement and the main functional component of nutritional supplements. It is similar to the function of phosphocreatine in the human body. Phosphate groups in muscles can participate in ADP The conversion to ATP provides energy for the body and increases muscle strength. At the same time, inositol phosphate can increase muscle volume, improve muscle flexibility and explosive power, and delay muscle fatigue. Because inositol phosphate is very soluble in water, can be directly absorbed and utilized by the human body, and has no toxic effects, it is more popular than protein products. With the rapid development of my country's sports industry, the demand for related sports functional foods will...

Claims

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Application Information

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IPC IPC(8): C07F9/09
CPCC07F9/091
Inventor 陈红余李平秦坤张煕曼
Owner TAISHAN MEDICAL UNIV
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