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Novel method for preparing high-purity creatine phosphate sodium

A technology of creatine phosphate sodium and a new method, which is applied in the field of preparing high-purity creatine sodium phosphate, can solve the problems of long production cycle, high production cost, complicated steps, etc., achieve short time consumption, reduce production cost, and improve safety Effect

Active Publication Date: 2012-07-11
ZHONGSHAN BAILING BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to improve the defects of complicated steps, long production cycle and high production cost in various production processes of high-purity creatine phosphate sodium, the present invention discloses a new method for preparing high-purity creatine phosphate sodium

Method used

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  • Novel method for preparing high-purity creatine phosphate sodium
  • Novel method for preparing high-purity creatine phosphate sodium
  • Novel method for preparing high-purity creatine phosphate sodium

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 1. Preparation of creatinine phosphate carboxylic acid mixed anhydride:

[0033] Add 100 mL of anhydrous ethyl acetate to a bottom flask, add 10.0 g (0.0435 mol) of creatinine phosphoryl chloride, stir and cool down to 0°C, and dissolve 14.5 g (0.0870 mol) of sodium isooctanoate in anhydrous acetic acid in another round bottom flask In 100mL of ethyl ester, keep 0-5°C and drop into the pre-cooled creatinine phosphoryl chloride, after adding, stir for 1 hour; filter, wash the filter cake with 20mL of anhydrous ethyl acetate, combine the filtrate and washing liquid to obtain creatinine phosphate carboxylic acid Ethyl acetate solution of mixed anhydride;

[0034] 2. Preparation of creatinine sodium phosphate:

[0035] The ethyl acetate solution of creatinine phosphate carboxylic acid mixed anhydride was maintained at 0°C, 35g of 20% sodium hydroxide was added dropwise at 0-5°C, stirred for 30 minutes, allowed to stand and separated, the ethyl acetate phase was extracted t...

example 2

[0039] 1. Preparation of creatinine phosphate carboxylic acid mixed anhydride:

[0040] Add 1000 mL of anhydrous ethyl acetate to a bottom flask, add 100.0 g (0.435 mol) of creatinine phosphoryl chloride, stir and cool down to 0°C, and dissolve 145.0 g (0.870 mol) of sodium isooctanoate in anhydrous acetic acid in another round bottom flask In 1000mL of ethyl ester, keep 0-5°C and drop into the pre-cooled creatinine phosphoryl chloride, after adding, stir for 1 hour; filter, wash the filter cake with 200mL of anhydrous ethyl acetate, combine the filtrate and washing liquid to obtain creatinine phosphate carboxylic acid Ethyl acetate solution of mixed anhydride;

[0041] 2. Preparation of creatinine sodium phosphate:

[0042] Keep the ethyl acetate solution of creatinine phosphate carboxylic acid mixed anhydride at 0°C, add 350.0g of 20% sodium hydroxide dropwise at 0-5°C, stir for 30 minutes, let stand to separate the layers, and extract the ethyl acetate phase with 350mL and...

example 3

[0046] 1. Preparation of creatinine phosphate carboxylic acid mixed anhydride:

[0047] Add 100 mL of anhydrous dichloroethane into the bottom flask, add 10.0 g (0.0435 mol) of creatinine phosphorus oxychloride, stir and cool down to 0 ° C, and dissolve 14.5 g (0.0870 mol) of sodium isooctanoate in anhydrous Dichloroethane 100mL, maintain 0-5 ℃, drop into the pre-cooled creatinine phosphorus oxychloride, add, stir for 1 hour; filter, wash the filter cake with 20mL anhydrous dichloroethane, combine the filtrate and lotion to obtain creatinine Dichloroethane solution of phosphoric acid carboxylic acid mixed anhydride;

[0048] 2. Preparation of creatinine sodium phosphate:

[0049] The dichloroethane solution of creatinine phosphate carboxylic acid mixed anhydride was maintained at 0°C, 35g of 20% sodium hydroxide was added dropwise at 0-5°C, stirred for 30 minutes, allowed to stand for stratification, and the dichloroethane phase was extracted with 35mL and 30mL of water respe...

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Abstract

The invention discloses a novel method for preparing high-purify creatine phosphate sodium. The preparation method comprises the following steps of: (1) generating fat-soluble creatinine phosphoric acid carboxylic acid mixed anhydride by using creatinine phosphorus oxychloride and carboxylate in an organic solvent; (2) making the creatinine phosphoric acid carboxylic acid mixed anhydride react with a sodium hydroxide aqueous solution, and crystallizing to obtain creatinine sodium phosphate; and (3) hydrolyzing the creatinine sodium phosphate in a sodium hydroxide aqueous solution for performing ring opening; neutralizing an organic carboxylic acid, and crystallizing to obtain creatine phosphate sodium. The prepared creatine phosphate sodium prepared with the method has high purity, high yield, simple purification steps, low time consumption, short production period; and heavy metals are not left in a product, and the safety of clinical administration is ensured.

Description

Technical field: [0001] The invention relates to a new method for preparing high-purity creatine phosphate sodium. Background technique: [0002] Phosphocreatine is a type of High Energy Phosphate Compounds , is a cardioprotective agent. [0003] Currently, creatine phosphate production methods include enzymatic synthesis, biological extraction and chemical synthesis. [0004] Although the conditions of enzymatic synthesis are mild, it is difficult to control, and the free enzyme protein also increases the difficulty of purification. [0005] The biological extraction method mainly extracts creatine phosphate from animal muscle tissue, but the content in the animal body is low, and the extraction cost is high. [0006] Chemical synthesis is currently a major way to produce creatine phosphate sodium. [0007] "Journal of Harbin University of Science and Technology" 2004, Volume 9, No. 4, had an article proposing to generate creatine phosphate by adding phosphorus oxychlor...

Claims

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Application Information

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IPC IPC(8): C07F9/22
Inventor 霍延豪张和平刘遗松阮宇峰梁待亮黄文军周海香黄凌沈惠宾
Owner ZHONGSHAN BAILING BIOTECHNOLOGY CO LTD
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