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Purification technology of dipyridamole

A technology of dipyridamole and purification method, which is applied in the field of pharmaceutical preparation and can solve the problems of difficulty in separating dipyridamole and the like

Active Publication Date: 2015-06-17
常州康普药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is: in the prior art, it is difficult to separate dipyridamole with higher purity from the crude product

Method used

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  • Purification technology of dipyridamole
  • Purification technology of dipyridamole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Put the solvent methanol and the dipyridamole crude product with an original purity of only 90% into the reaction pot at a mass ratio of 3.6:1, heat it in a water bath to 50°C, keep stirring and mix for 0.5 hours, and then add p-toluenesulfonate Acid and 1-(3-aminophenyl)-3-methyl-2-imidazolinone, the mass ratio of p-toluenesulfonic acid and dipyridamole crude product is 1:1, 1-(3-aminophenyl The mass ratio of )-3-methyl-2-imidazolinone to p-toluenesulfonic acid is 0.2:1; stir to dissolve it completely; cool the solution to 6°C, keep it warm for 2.5 hours, centrifuge the material, and dry it , washed with methanol, centrifuged again to shake off the material, and dried to obtain the sulfonate intermediate product;

[0018] (2) Mix the sulfonate intermediate product obtained in step (1) with 70% (solute mass fraction) methanol solution at a mass ratio of 1:6, heat and dissolve at 50°C to form a homogeneous solution, and heat at 50°C Insulate for 0.5 hours, add liqui...

Embodiment 2

[0021] (1) Put the solvent methanol and the dipyridamole crude product with an original purity of only 87.5% into the reaction pot at a mass ratio of 3.6:1, heat it in a water bath to 50° C., keep stirring and mix for 0.5 hours, and then add p-toluenesulfonate Acid and 1-(3-aminophenyl)-3-methyl-2-imidazolinone, the mass ratio of p-toluenesulfonic acid and dipyridamole crude product is 1:1, 1-(3-aminophenyl The mass ratio of )-3-methyl-2-imidazolidinone to p-toluenesulfonic acid is 0.2:1; stir to dissolve it completely; cool the solution to 8°C, keep it warm for 3 hours, centrifuge the material, and dry it , washed with methanol, centrifuged again to shake off the material, and dried to obtain the sulfonate intermediate product;

[0022] (2) Mix the sulfonate intermediate product obtained in step (1) with 70% (solute mass fraction) methanol solution at a mass ratio of 1:5, heat and dissolve at 50°C to form a homogeneous solution, and Insulate for 0.5 hours, add liquid alkali ...

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Abstract

The invention belongs to the field of drug preparation and particularly relates to a purification technology of a synthetic drug. The method comprises the steps of adding a methanol solvent and a dipyridamole crude product into methyl benzenesulfonic acid and 1-(3-aminobenzene)-3-methyl-2-imidazolone, stirring for reaction to form a sulfonate intermediate product, mixing the sulfonate intermediate product and a 70% methanol solution for dissolving, adding alkaline liquor to regulate pH (potential of hydrogen) of a system to 8-8.5, then adding active carbon, carrying out heating, decoloring, stirring and press filtration, cooling filtrate, and carrying out centrifuge, washing and drying to form purified high-purity dipyridamole.

Description

technical field [0001] The invention belongs to the field of medicine preparation, in particular to a purification process of synthetic medicine. Background technique [0002] The chemical name of dipyridamole is 2,2',2",2"'-[4,8-dipiperidinylpyrimido[5,4-d]pyrimidin-2,6-diyl]dinitrogen Base]-tetraethanol, molecular formula: C 24 h 40 N 8 o 4 , the molecular weight is 504.63, and the chemical structural formula is as follows: [0003] [0004] It is yellow crystalline powder; odorless, slightly bitter taste. Soluble in chloroform, soluble in ethanol, almost insoluble in water; soluble in dilute acid, melting point is 162-168°C. [0005] Dipyridamole has antithrombotic effects. Dipyridamole inhibits platelet aggregation, and high concentrations (50 μg / ml) can inhibit platelet release. The mechanism of action may be (1) inhibiting the uptake of adenosine by platelets, epithelial cells and red blood cells, and the inhibitory effect is dose-dependent at therapeutic co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
Inventor 王苏南汤金春
Owner 常州康普药业有限公司
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