A kind of preparation method of inositol phosphate

A technology of myo-inositol phosphate and myo-inositol phosphate, which is applied in the field of preparation of myo-inositol phosphate, can solve problems such as lack of solutions, and achieve the effects of easy biochemical treatment, convenient control of process parameters, and low emission

Active Publication Date: 2019-07-19
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of preparation method of inositol phosphate
  • A kind of preparation method of inositol phosphate
  • A kind of preparation method of inositol phosphate

Examples

Experimental program
Comparison scheme
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 method for preparing inositol phosphate, which comprises the following steps: after mixing ethyl acetate, inositol phosphate, p-toluenesulfonic acid and dicyclohexylcarbodiimide evenly, heating and refluxing reaction to obtain inositol phosphate alcohol crystals. P-toluenesulfonic acid acts as a catalyst to catalyze the esterification of inositol and phosphoric acid in inositol phosphate. Dicyclohexylcarbodiimide (DCC) is used as a dehydrating agent to remove the water generated by the esterification reaction, so that the whole reaction is carried out thoroughly and the reaction yield is improved. At the same time, the reaction solvent ethyl acetate can be recycled, and the by-products and impurities generated during the reaction remain in the ethyl acetate mother liquor, and the remaining dicyclohexylcarbodiimide (DCC) absorbs water to produce 1,3-bicyclic Hexylurea (DCU), which is insoluble in water, is easy to separate and purify during the recrystallization process, effectively ensuring product purity.

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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Patent Type & Authority Patents(China)
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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