Method for extracting croatine phosphate disodium salt from reaction solution

A technology of creatine phosphate disodium salt and reaction solution, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem that high-purity creatine phosphate disodium salt cannot be obtained, etc. problem, to achieve the effect of low production cost and simple method

Inactive Publication Date: 2010-06-09
SHANGHAI QICHENG PHARMA CO LTD
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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that high-purity creatine phosphate disodium salt cann...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: The 1st refining product of elution extraction

[0013] In the three-necked reaction flask, add 20 g of sodium hydroxide to hydrolyze the ring-opening reaction solution, add 100 g of isopropanol, stir at room temperature for 2 hours, and filter with suction to remove the precipitated sticky matter. The mother liquor was transferred to another three-necked reaction flask, stirred for 5 hours, filtered with suction, and the mother liquor was recovered. The wet weight of the filter cake is 6.1g, which is the refined product of phosphocreatine disodium salt for the first time of elution extraction.

Embodiment 2

[0014] Embodiment 2: the 2nd refining product of elution extraction

[0015] In the three-necked reaction flask, add 6.1 g of the refined product from the previous step, add 12.2 g of pure water, add 48.8 g of isopropanol, stir at room temperature for 2 hours, and suction filter to remove the precipitated sticky matter. The mother liquor was transferred to another three-necked reaction flask, stirred for 5 hours, filtered with suction, and the mother liquor was recovered. The wet weight of the filter cake is 5.2g, which is the refined product of creatine phosphate disodium salt for the second time of elution extraction.

Embodiment 3

[0016] Embodiment 3: the 3rd refining product of elution extraction

[0017] In the three-necked reaction flask, add 5.2g of the refined product from the previous step, add 10.4g of pure water, add 41.6g of isopropanol, stir at room temperature for 6 hours, suction filter, and recover the mother liquor. The filter cake was vacuum-dried to a constant weight to obtain 3.8 g of the product, which was elution extraction of disodium creatine phosphate hexahydrate. HPLC assay content 99.1%.

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Abstract

The invention provides a method for extracting croatine phosphate disodium salt from reaction solution. The method comprises the following steps of: reacting creatinine and an excessive amount of phosphorus oxychloride, performing hydrolysis and ring opening of the reaction product in solution of sodium hydroxide to obtain reaction solution, adding one or more solvents of monohydroxyl alcohol to the reaction solution, stirring the reaction solution for some time, extracting impurities generated by the side reaction, transferring mother liquor, extracting the product, performing the solid-liquid separation to obtain the first-time refined product, repeating the steps, and performing elution purification for several times to obtain the pharmaceutical grade croatine phosphate disodium salt. The method provided by the invention has the advantages of simpleness, low production cost, high product purity, and the suitability for industrialized production.

Description

technical field [0001] The invention relates to the field of chemical engineering separations. More specifically, it relates to a solvent-assisted elution to separate the inorganic polyphosphate and organic phosphate impurities in the creatine phosphate disodium salt solution after the reaction, thereby extracting pharmaceutical grade creatine phosphate disodium salt method. Background technique [0002] In order to obtain high-purity creatine phosphate disodium salt product and make the product suitable for powder injection, the purification process is a key process step for preparing creatine phosphate disodium salt. In the previous synthesis process, toxic barium salt was often used to remove phosphorus-containing impurities produced by side reactions. Reagents or procedures with high risk. Therefore, industrial production needs an effective method for removing side reaction phosphorus-containing impurities, so as to solve the bottleneck problem of preparing high-purit...

Claims

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Application Information

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IPC IPC(8): C07F9/22
Inventor 郁云忠张秋华郁春辉
Owner SHANGHAI QICHENG PHARMA CO LTD
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