Ilaprazole crystal form II and preparation method thereof

A technology of ilaprazole crystal and crystal form, which is applied in the field of ilaprazole crystal form and its preparation, and can solve problems such as poor stability, low drug efficacy, and insufficient properties of crystal form X

Inactive Publication Date: 2017-05-31
珠海保税区丽珠合成制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, CN101687849A describes ilaprazole solvate and its preparation method, including 1,4-dioxane racemic ilaprazole hemisolvate crystal C, tetrahydrofuran racemic ilaprazole hemisolvate Crystal D, methanol racemic ilaprazole hemisolvate crystal G, racemic ilaprazole hydrate crystal K; patent CN101687848A describes the crystal forms A, B, E, F, and I of ilaprazole and Its preparation method; the patent CN103172618B describes the X crystal form of ilaprazole and its preparation method. According to its description, the A, B, E, F, and I crystal forms have problems such as low drug efficacy and poor stability. However, in practice In the process, the properties of crystal form X disclosed by CN103172618B still have deficiencies

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve ilaprazole (10g) in a mixed solvent of dichloromethane (100ml) and methanol (100ml), concentrate and dry into an oil, add dichloromethane (50ml), acetone (50ml), dissolve, add ether (80ml ), 25°C, crystallization for 2 hours. Filter and dry to obtain type II crystals of ilaprazole, the product is 6.8 g, and the yield is 68%.

[0031] Bruker D8 Advance diffractometer was used to measure ilaprazole type II crystals, the results are shown in the appendix figure 1 , with the following conditions:

[0032] Instrument model: Bruker D8 Advance

[0033] Test conditions: X-ray source: Cu K

[0034] Working electricity: 40mA

[0035] Working voltage: 40KV

[0036] Detector: PSD

[0037] Start angle: 4°(2-theta)

[0038] Stop angle: 40°(2-theta)

[0039] Increment: 0.05° / step

[0040] Scan speed: 1sec / step

[0041] The results are characterized in Table 1 below:

[0042] Table 1

[0043]

[0044]

[0045] Differential scanning thermal analysis (DSC, in...

Embodiment 2

[0048] Dissolve ilaprazole (10g) in a mixed solvent of dichloromethane (100ml) and methanol (10ml), concentrate and dry into an oil, add dichloromethane (50ml), acetone (50ml), dissolve, add ether (80ml ), 25°C, crystallization for 2 hours. Filter and dry to obtain type II crystals of ilaprazole, the product is 6.2 g, the yield is 62%, and the purity is 99.9%.

Embodiment 3

[0050] Dissolve ilaprazole (10g) in a mixed solvent of dichloromethane (100ml) and acetone (10ml), concentrate and dry into an oil, add dichloromethane (50ml), acetone (50ml), dissolve, add ether (80ml ), 25°C, crystallization for 2 hours. Filter and dry to get the type II crystal of ilaprazole, the product is 6g, the yield is 60%, and the purity is 99.9%

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Abstract

The invention provides a novel Ilaprazole crystal form II. The novel Ilaprazole crystal form II is characterized in that an X-ray powder diffraction pattern has diffraction peaks at following 2-Theta degrees: 8.2+ / -1, 8.7+ / -1, 13.5+ / -1, 15.9+ / -1, 20.4+ / -1, 21.1+ / -1, 25.3+ / -1, 26.9+ / -1 and 28+ / -1. The crystal form is good in stability.

Description

technical field [0001] The invention belongs to the field of medicine, and relates to a crystal form of ilaprazole and a preparation method thereof. Background technique [0002] The structure of Ilaprazole (Ilaprazole) 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 transformed into an active metabolite of sulfenamide, which interacts with the sulfhydryl group on the H+, K+-ATPase to form a covalent combination of disulfide bonds, irreversibly inhibiting H+, K+- ATPase, which produces the effect of inhibiting gastric acid secretion. [0003] First-generation PPIs have limited clinical application because they can cause delayed gastric emptying, parietal cell swelling, and apparent rebound of gastric acid secretion after drug withdrawal. Ilaprazole, as one of the new generation of proton pump inhibitors (PPI), has overcome some of the defects o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14
CPCC07D401/14C07B2200/13
Inventor 肖鸿李桂铤李显焕戴奇志
Owner 珠海保税区丽珠合成制药有限公司
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