Polymorphism preparation method and application of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine

A technology of chlorophenoxy and phthalazine, which is applied in the field of polymorph preparation of 6-tetrazolo[5,1-a]phthalazine, which can solve the problems of no crystal form research reports and achieve reproducibility Good, simple operation effect

Inactive Publication Date: 2014-05-28
JILIN YINGLIAN SHANGDE SCI & TECH DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine is in the early stage of development as an antiepileptic drug, and there is no research report on its crystal form

Method used

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  • Polymorphism preparation method and application of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine
  • Polymorphism preparation method and application of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine
  • Polymorphism preparation method and application of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Preparation of Example 16-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine A crystal form

[0058] At 80°C, add 1g of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine into 20mL of acetonitrile solvent, slowly add the solvent until completely dissolved, and rapidly cool down to 0°C . The precipitated crystals were filtered, washed with a small amount of acetonitrile, and dried at 50° C. to obtain 0.82 g of white crystalline powder (type A), with a yield of 82%.

Embodiment 2

[0059] Example 26-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine A crystal preparation

[0060] At 60°C, add 1g of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine into 20mL of acetone solvent, slowly add the solvent until completely dissolved, and quickly cool down to 0°C . The precipitated crystals were filtered, washed with a small amount of acetone, and dried at 50° C. to obtain 0.67 g of a white crystalline solid (Type A), with a yield of 67%.

Embodiment 3

[0061] Preparation of Example 36-(4-Chlorophenoxy)-tetrazolo[5,1-a]phthalazine Form B

[0062] Suspend 1 g of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine in 40 mL of methanol solvent at 50°C, and stir the suspension with a magnetic stirring bar at 200 rpm After stirring for 2 days, the above suspension was filtered, washed with a small amount of methanol, and dried at room temperature to obtain 0.84 g of a white crystalline solid (type B), with a yield of 84%.

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Abstract

The invention discloses a polymorphism preparation method and an application of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine. New crystal forms are comprehensively characterized by utilizing X-ray powder diffraction, thermogravimetic analysis, differential scanning calorimetry, infrared, Raman, hygroscopic analysis and the like. The stability, the hygroscopic property and the dissolvability of four new crystal forms are compared, and references are provided for selecting a best solid form of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine used in medicine development. The new crystal form preparation method of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine has the advantages of simplicity, easy control, good reappearance, and stable obtaining of target crystal forms.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and relates to a polymorphic preparation method and application of 6-(4-chlorophenoxy)-tetrazolo[5,1-a]phthalazine. Background technique [0002] The current research on crystals has found that the same compound can exist in two or more crystalline states. When the molecular structure is the same but the crystal form is different, it may have different bioavailability, solubility, dissolution rate, melting point, color, filterability, density, fluidity and mechanical stability, etc. These physical and chemical properties or processability are sometimes directly affect the safety and effectiveness of the drug. Therefore, crystal form research and control has become an important research content in the process of drug development. [0003] Crystal form research includes two stages of crystal discovery and crystal form optimization. In the crystal discovery stage, various crystallization methods...

Claims

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Application Information

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IPC IPC(8): C07D487/04A61K31/5025A61P25/08
CPCC07D487/04A61P25/08
Inventor 全哲山李伟芦志刚于赢洲邓先清
Owner JILIN YINGLIAN SHANGDE SCI & TECH DEV
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