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Preparation method for medicine-istradefylline crystal form II for treating Parkinson

A technology for itraphylline and medicine is applied in the field of preparation of itraphylline crystal form II for treating Parkinson's disease, and can solve the problems of different stability, fluidity and compressibility, influence on drug efficacy, difference in bioavailability and the like. , to achieve the effect of improving quality, improving bioavailability, high yield and purity

Inactive Publication Date: 2018-06-01
董丹丹
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As we all know, the same drug has different crystal forms, and its bioavailability may also be different. In addition, its stability, fluidity, and compressibility may also be different. These physical and chemical properties have a certain impact on the application of the drug, thereby affecting drug efficacy

Method used

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  • Preparation method for medicine-istradefylline crystal form II for treating Parkinson
  • Preparation method for medicine-istradefylline crystal form II for treating Parkinson

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add istradefylline (10g) with a purity greater than 99.6% into a mixed solvent of isopropanol (20ml) and methyl tert-butyl ether (20ml), then heat to 70°C to dissolve, and quickly cool down to 1°C after dissolution , crystallization, that is, the drug istradefylline crystal form II for the treatment of Parkinson's is obtained.

[0031] The Parkinson's drug istradefylline crystal form II prepared in Example 1 was subjected to X-ray powder diffraction test to obtain the Parkinson's drug istradefylline crystal form II at diffraction angles 2θ at 8.687 degrees, 11.683 degrees and 12.120 degrees There are obvious diffraction peaks.

[0032] The optical purity of the istradefylline crystal form II of the Parkinson's drug prepared in Example 1 was determined:

[0033] Take the istradefylline crystal form II of the drug for treating Parkinson’s prepared in Example 1, accurately weigh 100 mg and place it in a 100 ml measuring bottle, add mobile phase to ultrasonically dissolve ...

Embodiment 2

[0055] (1) Dissolve the reaction raw material 1,2-dimethoxybenzene (A) (20g, 8.2mol) and ethylene (22.5g, 9.84mol) in acetonitrile (80ml), add aluminum trichloride (2.5g) , stir well, control the reaction temperature at 127°C, and the reaction pressure at 0.2Mpa, use the liquid phase method to react 1,2-dimethoxybenzene (A) with ethylene in the tower reactor, and the reaction ends;

[0056] (2) Put the reaction solution in step (1) in a vertical reactor, add catalyst iron oxide (1.2g) and cocatalyst potassium (0.6g), add a large amount of high-temperature water vapor at 560°C, continue the reaction, and form E-2-(3,4-dimethoxy)styrene (B) (35.16g, 12.42mol);

[0057] (3) Combine E-2-(3,4-dimethoxy)styrene (B) (35.16g, 12.42mol) produced in step (2) with 1,3-diethyl-8-iodo-7 -Methylpurine-2,6-dione (C) (36.2g, 14.28mol) was mixed and dissolved in N,N-dimethylformamide (DMF) (100ml), and N,N-diisopropyl Ethylamine (40g, 14.9mol), tri-o-tolylphosphine (3.6g, 1.2mol) and palladi...

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Abstract

The invention discloses a preparation method for a medicine-istradefylline crystal form II for treating Parkinson. After the istradefylline and mixed solvent are mixed, mixture is heated to 70-90 DEGC to be dissolved, then, the mixture is quickly cooled to 0-5 DEG C, and crystallization is carried out to obtain the istradefylline crystal form II for treating Parkinson. The stability of the istradefylline crystal form II for treating Parkinson is equivalent to the stability of the traditional istradefylline crystal form II, yield and purity are higher, the quality of a product is greatly improved, in addition, the bioavailability of the istradefylline crystal form II can be improved so as to be favorable for the medicine processing and user in a medicine composite, and meanwhile, qualitative and quantitative information can be provided so as to have an important meaning for further researching the curative effect of the solid medicine.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis of medicines, and in particular relates to a preparation method of crystal form II of istradefylline, a drug for treating Parkinson's. Background technique [0002] Itradefylline (Istradefylline, KW6002), the chemical name is 8-[(E)-2-(3,4-dimethoxyphenyl)vinyl]-1,3-diethyl-7-methyl Purine-2,6-dione, the structural formula is as follows: [0003] . [0004] Itradefylline is a selective adenosine A2a receptor antagonist, which can improve the motor function of patients with Parkinson's disease by changing the activity of neurons. Patent No. CN201510012448.X discloses the crystal form of istradefylline, and its process route is: [0005] . [0006] Patent No. CN201510012448.X uses 8-[(E)-2-(3,4-dimethoxyphenyl)vinyl]-1,3-diethyl-7-hydrogen-purine-2,6- Diketone is used as a raw material, and methyl iodide is heated and reacted under the action of potassium carbonate to generate istradefylli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/06
CPCC07D473/06C07B2200/13
Inventor 董丹丹
Owner 董丹丹
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