Preparation method and application of spherical crystal of disodium adenosine triphosphate

A technology of disodium adenosine triphosphate and spherical crystals, applied in the field of medicine, can solve the problems of difficult suction filtration and drying, thin crystals, loose aggregates and the like

Pending Publication Date: 2022-05-31
苏州赜文医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adenosine triphosphate disodium is usually a white powdery solid. After crystallization, flaky crystals will be obtained. The crystals are thin and easy to aggregate, which makes it difficult to filter and dry after crystallization, which poses challenges to downstream production.
However, for disodium adenosine triphosphate, no patents and documents have been found to report on the preparation process of spherical crystals, and due to the crystal nucleation and growth properties of disodium adenosine triphosphate itself, it is easy to explode nucleation, crystal growth is flake, and it is easy to coalesce to form a solvent Occluded, but its aggregates are often loose and irregular

Method used

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  • Preparation method and application of spherical crystal of disodium adenosine triphosphate
  • Preparation method and application of spherical crystal of disodium adenosine triphosphate
  • Preparation method and application of spherical crystal of disodium adenosine triphosphate

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preparation example Construction

[0068] Preparation method of adenosine triphosphate disodium spherical crystal

[0069] In order to overcome the defects in the prior art, the present invention provides a novel method for preparing spherical adenosine triphosphate disodium crystals. The spherical adenosine triphosphate disodium crystals prepared by the method have low bulk density, good fluidity, high purity and uniform particle size.

[0070] Typically, the present invention provides a method for preparing spherical crystals of adenosine triphosphate disodium shown in formula (I), comprising the steps of:

[0071] (1) providing disodium adenosine triphosphate raw material in water, stirring and preparing disodium adenosine triphosphate aqueous solution, wherein the disodium adenosine triphosphate aqueous solution is a saturated or supersaturated aqueous solution with a mass fraction of 5-42%;

[0072] (2) crystallization, described crystallization step is carried out by (Ia)-(Ib):

[0073] (Ia) Adjust the t...

Embodiment 1

[0121] At room temperature, add 12.6 g of adenosine triphosphate disodium raw material into 56.5 mL of water to prepare about 20% adenosine triphosphate disodium aqueous solution. Stir at 250rpm, add 138mL of absolute ethanol dropwise to the aqueous solution at 45°C at a rate of about 1.3mL / min, when it reaches 12mL, fine crystals precipitate out of the solution, the solution is slightly cloudy, and the dropwise addition is suspended. The temperature of the solution was lowered to 30°C, and the dropwise addition was continued after keeping the temperature for 10 minutes.

[0122] After the dropwise addition, keep warm for 1h. Subsequently, the temperature was lowered to 20°C at a rate of 10°C / h, and then kept for 30 minutes, and then the material was collected.

[0123] After vacuum filtration, the filter cake was washed with about 145 mL of absolute ethanol, and the filtration speed was fast to obtain 17.8 g of wet product. After vacuum drying at 35°C, 12.3 g of dry product...

Embodiment 2

[0126] At room temperature, add 12.6 g of adenosine triphosphate disodium raw material into 113 mL of water to prepare about 10% adenosine triphosphate disodium aqueous solution. Stir at 250rpm, add 276mL of absolute ethanol dropwise to the aqueous solution at 45°C at a rate of about 1.3mL / min. When the solution reaches about 27mL, fine crystals will precipitate out of the solution, and the solution will be slightly cloudy, so stop the dropwise addition. The temperature of the solution was lowered to 30°C, and the dropwise addition was continued after keeping the temperature for 10 minutes.

[0127] After the dropwise addition, keep warm for 1h. Subsequently, the temperature was lowered to 20°C at a rate of 10°C / h, and then kept for 30 minutes, and then the material was collected.

[0128] After vacuum filtration, the filter cake was washed with about 142 mL of absolute ethanol, and the filtration speed was fast to obtain 20.7 g of wet product. After vacuum drying at 35°C, 1...

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Abstract

The invention provides a preparation method and application of a spherical crystal of disodium adenosine triphosphate. Specifically, the invention provides a spherical crystal of a compound as shown in a formula I. The crystal is uniform in particle size, high in purity, good in fluidity, not prone to coalescence, high in bulk density and convenient to separate and dry.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a preparation method and application of spherical crystals of adenosine triphosphate disodium. Background technique [0002] Adenosine triphosphate disodium, chemical name: adenosine-5'-triphosphate disodium salt, molecular formula: C 10 h 14 N 5 Na 2 o 13 P 3 , the molecular weight is 551.09, and the structural formula is as follows. [0003] [0004] Adenosine triphosphate disodium is a derivative of nucleotides and is a coenzyme that participates in the metabolism of fat, protein, sugar, nucleic acid, and nucleotides in the body. Adenosine triphosphate disodium can penetrate the blood-brain barrier, improve the stability and reconstruction ability of nerve cell membrane structure, and promote nerve growth. It is clinically used for various diseases caused by tissue damage and decreased cellular enzyme activity. [0005] Patent 200710019776.8 discloses a productio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/06C07H19/20A61K31/7076A61P25/00
CPCC07H1/06C07H19/20A61P25/00C07B2200/13
Inventor 李娟郑新华
Owner 苏州赜文医药科技有限公司
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