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Ilaprazole crystal form and preparation method thereof

A technology of ilaprazole crystal and crystal form, applied in the field of ilaprazole crystal form and preparation thereof, can solve the problems of poor stability, low efficacy and the like, and achieve the effects of good stability, easy preparation and low impurity content

Active Publication Date: 2013-06-26
LIVZON PHARM GRP INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Patent CN101687848A discloses A, B, E, F, and I crystal forms of the ilaprazole compound shown in formula (I), but the above crystal forms still have the problems of low drug efficacy and poor stability, etc.

Method used

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  • Ilaprazole crystal form and preparation method thereof
  • Ilaprazole crystal form and preparation method thereof
  • Ilaprazole crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] At 25°C, add 10g of ilaprazole to a 250ml single-necked flask, add 100ml of dichloromethane and 100ml of anhydrous methanol successively, stir the solution until the ilaprazole is completely dissolved, and then transfer the solution to a constant pressure funnel. The above-mentioned ilaprazole mixed solution is slowly added dropwise to 250ml of ether, and the temperature of the reaction system is controlled within the range of 25±2°C during the dropping process, and the dropping time is controlled between 25 and 30 minutes. After the addition was completed, the temperature was kept at 25°C and the solution was stirred for 40 minutes to crystallize. Vacuum filtration under reduced pressure, washing the filter cake with 150 ml of ether, and vacuum drying at room temperature for 24 hours to obtain an off-white powder, ilaprazole crystal form X, with a yield of 85%.

[0036] The Bruker D8Advance diffractometer was used to determine the X-ray powder diffraction pattern of ilapr...

Embodiment 2

[0047] At 25° C., 1 kg of ilaprazole was added to the reaction tank, 10L of dichloromethane and 10L of anhydrous methanol were added in sequence, the solution was stirred until the ilaprazole was completely dissolved, and then the solution was transferred to the metering tank. The above-mentioned ilaprazole mixed solution is slowly added to 25L of ether, and the temperature of the reaction system is controlled within the range of 25±2°C during the dropping process, and the dropping time is controlled between 25-30 min. After the addition was completed, the solution was stirred at 25°C for 40 minutes to crystallize. Vacuum filtration was performed under reduced pressure, the filter cake was washed with 15 L of ether, and dried under vacuum at room temperature for 24 hours to obtain an off-white powder of crystal form X with a yield of 88.8%.

[0048] After testing, the analysis result of ilaprazole crystal form X prepared in Example 2 is not significantly different from the analys...

Embodiment 3

[0050] At 25°C, add 10g of ilaprazole to a 250ml single-necked flask, add 100ml of chloroform and 100ml of absolute ethanol in sequence, stir the solution until the ilaprazole is completely dissolved, and then transfer the solution to a constant pressure funnel. The above-mentioned ilaprazole mixed solution is slowly added dropwise to 250ml of ether, and the temperature of the reaction system is controlled within the range of 25±2°C during the dropping process, and the dropping time is controlled between 25 and 30 minutes. After the addition was completed, the solution was stirred at 25°C for 40 minutes to crystallize. Vacuum filtration was performed under reduced pressure, the filter cake was washed with 150 ml of ether, and dried under vacuum at room temperature for 24 hours to obtain an off-white powder of crystal form X with a yield of 87%.

[0051] After testing, the analysis result of ilaprazole crystal form X prepared in Example 3 is not significantly different from the an...

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Abstract

The invention discloses an ilaprazole crystal form X and a preparation method thereof. The ilaprazole crystal form X disclosed by the invention is easy to prepare. The ilaprazole crystal form X provided by the invention is high in purity and low in impurity content. The preparation method disclosed by the invention is low in required solvent amount and low in production cost. The preparation method is simple to operate, mild in reaction conditions, easy to control, and can obtain a target product crystal form in an extremely determined and good-reproducibility mode.

Description

Technical field [0001] The invention belongs to the field of medicine and relates to an ilaprazole crystal form and a preparation method thereof. Background technique [0002] Ilaprazole (Ilaprazole) structure belongs to the benzimidazole class and is an irreversible proton pump inhibitor. After oral administration, ilaprazole selectively enters the parietal cells of the stomach and is converted into the active metabolite of sulfenamide. + , K + -The sulfhydryl group on the ATPase forms the covalent bond of the disulfide bond, irreversibly inhibits H + , K + -ATPase, which inhibits the secretion of gastric acid. [0003] The first generation of PPI has limitations in clinical application because it can cause delayed gastric emptying, parietal cell swelling, and obvious gastric acid secretion rebound after drug withdrawal. As one of the new generation of proton pump inhibitors (PPI), ilaprazole has overcome some of the shortcomings of the original similar products to varying degree...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14A61K31/4439A61P1/04
Inventor 侯雪梅周月广曾创毛文金李菁
Owner LIVZON PHARM GRP INC
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