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Trihydrate crystal of disodium adenosine triphosphate and preparation method thereof

A technology of adenosine triphosphate disodium trihydrate and adenosine triphosphate disodium trihydrate, which is applied in the field of medicine and can solve the problems of unfavorable industrial production and storage, complex preparation process, and low crystallinity

Pending Publication Date: 2022-05-27
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

At present, the adenosine triphosphate disodium drug substance on the market has poor stability, low crystallinity, easy moisture absorption, complex preparation process, and is not conducive to industrial production and storage.

Method used

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  • Trihydrate crystal of disodium adenosine triphosphate and preparation method thereof
  • Trihydrate crystal of disodium adenosine triphosphate and preparation method thereof
  • Trihydrate crystal of disodium adenosine triphosphate and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment approach

[0063] In a preferred embodiment, the crystal also has one or more X-ray powder diffraction characteristic peaks selected from the following group: 13.9°±0.2°, 27.3°±0.2°, 15.2°±0.2° , 26.8°±0.2°, 29.6°±0.2°, 21.4°±0.2°, 25.6°±0.2°, 21°±0.2°, 15.7°±0.2°, 31°±0.2°, 25°±0.2°, 30.6 °±0.2°, 26.2°±0.2°, 13.5°±0.2°, 16.2°±0.2°, 28.6°±0.2°, 33.6°±0.2°, 36.6°±0.2°, 34°±0.2°, 33.1°± 0.2°, 38.8°±0.2°, 37.2°±0.2°, 39.7°±0.2°.

[0064] In another preferred embodiment, the crystal has X-ray powder diffraction characteristic peaks selected from the following group: 17.2°±0.2°, 5.6°±0.2°, 18.7°±0.2°, 23.1°±0.2° , 11.5°±0.2°, 13.9°±0.2°, 27.3°±0.2°, 15.2°±0.2°, 26.8°±0.2°, 29.6°±0.2°, 21.4°±0.2°, 25.6°±0.2°, 21 °±0.2°, 15.7°±0.2°, 31°±0.2°, 25°±0.2°, 30.6°±0.2°, 26.2°±0.2°, 13.5°±0.2°, 16.2°±0.2°, 28.6°± 0.2°, 33.6°±0.2°, 36.6°±0.2°, 34°±0.2°, 33.1°±0.2°, 38.8°±0.2°, 37.2°±0.2°, 39.7°±0.2°.

[0065] In another preferred embodiment, the crystals have X-ray powder diffraction characteristic...

Embodiment 1

[0100] At room temperature, 2.00 g of adenosine triphosphate disodium raw material was added to 8 mL of water to prepare a 20% aqueous solution. Under stirring, 25 mL of absolute ethanol was added dropwise to the 60° C. aqueous solution, and the stirring speed was 250 rpm. After the dropwise addition, the solution was cooled to 30°C, and a solid was precipitated. After suction filtration, the filter cake was washed with about 20 mL of absolute ethanol, and dried under vacuum at 25°C to obtain 1.62 g of dry product adenosine disodium triphosphate trihydrate crystal, the total yield was 81.0%, and the purity measured by HPLC was 99.24%.

[0101] The obtained crystals of adenosine triphosphate disodium trihydrate were tested by XRPD, and the results were as follows figure 1 The spectral data are shown in Table A. TGA test was carried out on the obtained solid, and the results were as follows figure 2 As shown, the results show that in the TGA spectrum of the adenosine triphos...

Embodiment 2

[0106] At room temperature, 1.01 g of adenosine triphosphate disodium raw material was added to 9 mL of water to prepare a 10% aqueous solution. Under stirring, 10 mL of acetone was added dropwise to the 40° C. aqueous solution, and the stirring speed was 250 rpm. After the dropwise addition, the solution was cooled to 30°C, and a solid was precipitated. After suction filtration, the filter cake was washed with about 10 mL of absolute ethanol, and dried in vacuum at 25°C to obtain 0.83 g of dry product adenosine disodium triphosphate trihydrate crystal, the total yield was 82.2%, and the purity measured by HPLC was 99.52%.

[0107] The obtained crystals of adenosine disodium triphosphate trihydrate were tested by XRPD, and the results were roughly as follows figure 1 shown. TGA test was performed on the obtained solid, and the result showed that in the TGA spectrum of the adenosine triphosphate disodium trihydrate crystal, the weight loss before decomposition was 8.921%.

...

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Abstract

The invention provides an adenosine disodium triphosphate trihydrate crystal and a preparation method thereof. Specifically, the invention provides a crystal of a compound as shown in a formula I, and the crystal is a trihydrate crystal. The crystal is high in stability, simple in preparation process, high in yield and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a trihydrate crystal of disodium adenosine triphosphate and a preparation method thereof. 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 shown below. [0003] [0004] Adenosine disodium triphosphate is a derivative of nucleotides and is a coenzyme involved in the metabolism of fat, protein, sugar, nucleic acid and nucleotides in the body. Adenosine disodium triphosphate 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 cell enzyme activity. [0005] Patent 200710019776.8 discloses a production method...

Claims

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Application Information

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IPC IPC(8): C07H19/20C07H1/06A61P25/00A61K31/7076
CPCC07H19/20C07H1/06A61P25/00C07B2200/13
Inventor 郑新华李娟
Owner 苏州赜文医药科技有限公司
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