Preparation method of creatine phosphate disodium dihydrate

A technology for creatine disodium phosphate dihydrate and creatine, which is applied in the field of preparation of creatine phosphate disodium disodium dihydrate, can solve the problems of low yield and purity, long reaction time, low production efficiency and the like, and achieves purity High effect, short preparation time and high production efficiency

Active Publication Date: 2014-08-20
TIANJUSHI ENG TECH GROUP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of disodium creatine phosphate dihydrate to solve the existing preparation methods with complex processes, long reaction time, low production efficiency, high toxicity of raw materials, relatively low yield and purity The problem

Method used

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  • Preparation method of creatine phosphate disodium dihydrate
  • Preparation method of creatine phosphate disodium dihydrate
  • Preparation method of creatine phosphate disodium dihydrate

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Dissolve 131g (1 mol) of creatine in 500 mL of anhydrous acetonitrile, and gradually add 200g (1.3 mol) of phosphorus oxychloride in an ice bath, and then slowly add 656g (6.5 mol) of catalyst triethylamine; under the condition of -4°C-0°C, stir for 30 min to make it fully react, carry out the reaction, and obtain the reaction liquid;

[0027] (2) Add 54 mL (3mol) of water to the reaction solution, stir for 5 min, then add 1500 mL of absolute ethanol, and wait until the crystals are fully separated;

[0028] (3) Filtrate, dry the filter cake at 40°C, add 500 mL of ethanol aqueous solution with a concentration of 95% by volume, raise the temperature to 60°C to fully dissolve it, then let it stand at room temperature to fully separate out the crystals, filter, and use the same Wash the filter cake twice with an aqueous ethanol solution at a concentration of 40°C, and dry the filter cake under vacuum at 40°C to obtain pure creatine phosphate;

[0029] (4) Dissolve the...

Embodiment 2

[0031] (1) Dissolve 131g (1 mol) of creatine in 500 mL of anhydrous acetonitrile, and gradually add 154 g (1 mol) of phosphorus oxychloride under ice-bath conditions, after dissolving, slowly add 606 g (6.0 mol) catalyst triethylamine; under the condition of -4°C-0°C, stir for 1 h to make it fully react, and react to obtain a reaction solution;

[0032] (2) Add 54 mL (3mol) of water to the reaction solution, stir for 5 min, then add 1500 mL of absolute ethanol, and wait until the crystals are fully separated;

[0033] (3) Filtrate, dry the filter cake at 35°C, add 500 mL of ethanol aqueous solution with a concentration of 98% by volume, raise the temperature to 60°C to fully dissolve it, then let it stand at room temperature to fully separate the crystals, filter, and use volume Wash the filter cake once with an aqueous ethanol solution with a specific concentration of 98%, and vacuum-dry the filter cake at 40°C to obtain pure creatine phosphate;

[0034] (4) Dissolve the pur...

Embodiment 3

[0036](1) Dissolve 131 g (1 mol) of creatine in 500 mL of anhydrous acetonitrile, and gradually add 230 g (1.5 mol) of phosphorus oxychloride under ice bath conditions, and then slowly add 808 g ( 8.0 mol) of catalyst triethylamine; under the condition of -4°C-0°C, stir for 0.5 h to make it fully react, carry out the reaction, and obtain the reaction solution;

[0037] (2) Add 54 mL (3mol) of water to the reaction solution, stir for 5 min, then add 1500 mL of absolute ethanol, and wait until the crystals are fully separated;

[0038] (3) Filtrate, dry the filter cake at 40°C, add 500 mL of ethanol aqueous solution with a concentration of 90% by volume, raise the temperature to 60°C to fully dissolve, then let it stand at room temperature to fully separate out the crystals, filter, and use the same Wash the filter cake twice with an aqueous ethanol solution of a certain concentration, and dry the filter cake under vacuum at 45°C to obtain pure creatine phosphate;

[0039] (4) ...

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Abstract

The invention discloses a preparation method of a creatine phosphate disodium dihydrate. The preparation method of the creatine phosphate disodium dihydrate comprises the following steps of: (a) dissolving creatine into anhydrous acetonitrile, adding phosphorus oxychloride and a triethylamine catalyst under the ice bath condition; stirring for full reaction, so as to obtain reaction liquid, wherein mole ratio of creatine to phosphorus oxychloride to triethylamine is 1:(1-1.5):(6-8); (b) adding water into the reaction liquid, hydrolyzing, then adding absolute ethyl alcohol, and separating out crystals; (c) filtering, drying a filter cake, adding ethanol water, and recrystallizing, so as to obtain pure creatine phosphoric acid; (d) dissolving the pure creatine phosphoric acid into ethanol water, adding sodium hydroxide, cooling, filtering to obtain a filter cake, dissolving the filter cake into the ethanol water, and recrystallizing, thus obtaining the pure creatine phosphate disodium dihydrate. The preparation method of the creatine phosphate disodium dihydrate has the advantages of small use amount of phosphorus oxychloride during preparation, high safety factor, low cost, high yield, high product purity, short preparation time, high production efficiency and easy operation and control and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of medical supplies, in particular to a preparation method of disodium creatine phosphate dihydrate. Background technique [0002] As a cardioprotective drug, creatine phosphate sodium salt has been widely used in the prevention and adjuvant treatment of various heart diseases such as myocardial ischemia, ventricular hypertrophy, myocardial infarction and heart failure. Its medical value ranks first among similar drugs. At present, the preparation methods of creatine phosphate sodium salt mainly include enzymatic method, biological extraction method and synthetic method. Among them, the enzymatic preparation of creatine phosphate sodium salt has the characteristics of mild reaction conditions, fast reaction rate and strong specificity, but the optimal conditions of the enzyme reaction are not easy to control, and it is difficult to remove the enzyme protein after the reaction, and the process operation is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/22
Inventor 刘哲封马忠青刘秀忠梁希娟王京史静宏姚振永陈钊
Owner TIANJUSHI ENG TECH GROUP
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