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Crystal form of diethanolamine salt of thrombopoietin mimic and preparation method thereof

A technology of crystallization and medicine, applied in the crystallization form of diethanolamine salt of thrombopoietin mimic and its preparation field, can solve problems such as easy agglomeration, poor product stability, difficult filtration, etc., and achieve repeatable and controllable production process, Good crystal form stability and stable production process

Inactive Publication Date: 2015-08-19
JIANGSU HENGRUI MEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally speaking, amorphous drug products have no regular crystal structure and often have other defects, such as poor product stability, fine crystallization, difficult filtration, easy agglomeration, poor fluidity, etc.

Method used

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  • Crystal form of diethanolamine salt of thrombopoietin mimic and preparation method thereof
  • Crystal form of diethanolamine salt of thrombopoietin mimic and preparation method thereof
  • Crystal form of diethanolamine salt of thrombopoietin mimic and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Take (1.0g, 2.2mmol) (Z)-5-(2-hydroxyl-3-(2-(3-methyl-5-oxo-1-(5,6,7,8-tetrahydronaphthalene- 2-yl)-1H-pyrazole-4(5H)-ylidene)hydrazino)phenyl)furan-2-carboxylic acid (prepared according to the method disclosed in WO2009092276), add 10mL methanol in an ice-water bath, and add, (266mg, 4.3mmol) ethanolamine was added dropwise, after the addition was completed, stirred at room temperature, a large amount of solids precipitated, stirred overnight, filtered, and dried to obtain 480mg of the compound represented by formula (I) as a solid, with a yield of 38%. The X-ray diffraction spectrum figure of this crystalline sample is shown in figure 1 . The crystallization at about 2.96 (29.86), 5.97 (14.80), 7.37 (11.98), 8.40 (10.52), 8.95 (9.87), 12.04 (7.35), 12.89 (6.86), 15.09 (5.87), 16.91 (5.24), 18.34 (4.83), 21.85(4.06), 22.64(3.92), 24.20(3.67) and 26.13(3.41) have characteristic peaks. See the DSC spectrum figure 2 , there is a melting endothermic peak around 159.53...

Embodiment 2

[0037] Take (1.0g, 2.2mmol) (Z)-5-(2-hydroxyl-3-(2-(3-methyl-5-oxo-1-(5,6,7,8-tetrahydronaphthalene- 2-yl)-1H-pyrazole-4(5H)-ylidene)hydrazino)phenyl)furan-2-carboxylic acid, add 10mL ethanol in ice-water bath, add dropwise (266mg, 4.3mmol) After the addition of ethanolamine, stir at room temperature, a large amount of solids precipitated, stirred overnight, filtered, and dried to obtain 806 mg of the compound represented by formula (I) as a solid, with a yield of 64%. Its X-diffraction and DSC patterns are researched and compared, and it is confirmed that the product is A crystal form.

Embodiment 3

[0039]Take (1.0g, 2.2mmol) (Z)-5-(2-hydroxyl-3-(2-(3-methyl-5-oxo-1-(5,6,7,8-tetrahydronaphthalene- 2-yl)-1H-pyrazole-4(5H)-ylidene)hydrazino)phenyl)furan-2-carboxylic acid, add 10mL isopropanol in an ice-water bath, add dropwise into (266mg, 4.3 mmol) ethanolamine, the addition was completed, stirred at room temperature, a large amount of solids precipitated, stirred overnight, filtered, and dried to obtain 800 mg of the compound shown in formula (I) as a solid, with a yield of 63%. Its X-diffraction and DSC patterns are researched and compared, and it is confirmed that the product is A crystal form.

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Abstract

The invention relates to a crystal form of a diethanolamine salt of a thrombopoietin mimic and a preparation method thereof. Specifically, the invention relates to a type A crystal of (Z)-5-(2-hydroxy-3-(2-(3-methyl-5-oxo-1-(5,6,7,8-tetralin-2-yl)-1H-pyrazole-4(5H)-idene)hydrazino)phenyl)furan-2-diethanolamine carboxylate (a compound as shown in a formula (I)) and a preparation method thereof. The crystal has an x-ray powder diffraction pattern as shown in a figure 1. The type A crystal of the compound as shown in the formula (I) has good chemical stability and crystal-form stability, uses a crystallization solvent with low toxicity and low residues and can be better applied to clinical treatment.

Description

technical field [0001] The present invention relates to (Z)-5-(2-hydroxyl-3-(2-(3-methyl-5-oxo-1-(5,6,7,8-tetrahydronaphthalene-2-yl)- Type A crystal of 1H-pyrazole-4(5H)-ylidene)hydrazino)phenyl)furan-2-carboxylic acid diethanolamine salt and its preparation method. Background technique [0002] Platelets are cells that play an important role in the process of stopping bleeding and repairing damaged blood vessels. A severe deficiency of platelets, known as thrombocytopenia, can have serious consequences and even death. Thrombocytopenia includes idiopathic thrombocytopenia purpura (ITP), and thrombocytopenia caused by chemotherapy (interferon IFN, heparin, etc.), radiotherapy, bacterial or viral infection (HIV, hepatitis C, etc.) and liver disease. [0003] Thrombopoietin (TPO) is a hematopoietic growth factor that stimulates platelet production in the body. It can regulate the proliferation, differentiation, and maturation of megakaryocytes by binding to a specific recept...

Claims

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Application Information

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IPC IPC(8): C07D405/12A61K31/4155A61P7/00
CPCC07D405/12
Inventor 武乖利高晓晖刁艾青吴玉霞
Owner JIANGSU HENGRUI MEDICINE CO LTD
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