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Ilaprazole crystal form and its preparation method and application

A technology of ilaprazole and its crystal form, which is applied in the field of new ilaprazole crystal form and its preparation, can solve the problems of poor stability and low drug efficacy, and achieve less solvent, easy preparation and good reproducibility Effect

Active Publication Date: 2016-05-18
HARBIN SANLIAN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Patent CN101687848B discloses A, B, E, F, and I crystal forms of ilaprazole compound, but the above crystal forms still have problems such as low drug efficacy and poor stability

Method used

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  • Ilaprazole crystal form and its preparation method and application
  • Ilaprazole crystal form and its preparation method and application
  • Ilaprazole crystal form and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1: Preparation of ilaprazole M crystal form

[0040] 1) Dissolve 1g ilaprazole in 10mL chloroform;

[0041] 2) Evaporate the above solution to dryness under reduced pressure below 30°C, add 10mL ethyl acetate after evaporation, dissolve, stir and crystallize for 30min;

[0042] 3) Filter the crystals, wash the filter cake three times with ethyl acetate, and dry at 28° C. to obtain 0.756 g of off-white crystalline powder with a yield of 75.6%.

[0043] The X-ray powder diffraction of the obtained ilaprazole M crystal form is: 7.047, 9.128, 11.758, 12.637, 14.752, 15.815, 18.119, 19.466, 20.189, 21.121, 22.080, 22.726, 23.614, 24.024, 24.415, There are characteristic peaks at 25.441, 27.028, 27.811, 28.860, and 31.347; 1 H-NMR (CDCl 3 ) data are: 8.33(d, 1H), 7.63(d, 1H), 7.45(s, 1H), 7.31(m, 1H), 7.15(s, 2H), 6.66(d, 1H), 6.36(s, 2H), 4.82(dd, 2H), 3.82(s, 3H), 2.11(s, 3H); its IR(KBr, cm -1 ) data are: 3425, 3187, 3106, 3059, 2966, 2933, 2885, 2830, 2561...

Embodiment 2

[0044] Embodiment 2: Preparation of ilaprazole M crystal form

[0045] 1) Dissolve 1g ilaprazole in 10mL chloroform and dissolve;

[0046] 2) Evaporate the above solution to dryness under reduced pressure below 30°C, add 15mL ethyl acetate after evaporation, and quickly dissolve in the dark, and stir and crystallize in the dark for 30 minutes after dissolution;

[0047] 3) Filter the crystals, wash the filter cake three times with ethyl acetate, and dry at 28°C. Obtained 0.758 g of off-white crystalline powder with a yield of 75.8%.

[0048] The X-ray powder diffraction of the obtained ilaprazole M crystal form is: 7.050, 9.120, 11.761, 12.635, 14.757, 15.810, 18.114, 19.461, 20.189, 21.116, 22.074, 22.731, 23.601, 24.028, 24.414, There are characteristic peaks at 25.439, 27.029, 27.806, 28.861, and 31.351; 1 H-NMR (CDCl 3 ) data are: 8.32(d, 1H), 7.65(d, 1H), 7.48(s, 1H), 7.34(m, 1H), 7.14(s, 2H), 6.65(d, 1H), 6.37(s, 2H), 4.83(dd, 2H), 3.80(s, 3H), 2.13(s, 3H); its IR(K...

Embodiment 3

[0050] 1) Dissolve 1g ilaprazole in 10mL chloroform, and dissolve quickly in the dark;

[0051] 2) Evaporate the above solution to dryness under reduced pressure below 30°C, add 20 mL of ethyl acetate after evaporation, and quickly dissolve in the dark, and stir and crystallize in the dark for 45 minutes after dissolution;

[0052] 3) Filter the crystals, wash the filter cake three times with ethyl acetate, and dry at 28°C. 8.67 g of off-white crystalline powder was obtained with a yield of 86.7%.

[0053] The X-ray powder diffraction of the obtained ilaprazole M crystal form is: 7.048, 9.119, 11.763, 12.632, 14.760, 15.812, 18.117, 19.465, 20.187, 21.119, 22.079, 22.733, 23.606, 24.030, 24.413, There are characteristic peaks at 25.440, 27.030, 27.808, 28.864, and 31.352; 1 H-NMR (CDCl 3 ) data are: 8.30(d, 1H), 7.67(d, 1H), 7.50(s, 1H), 7.37(m, 1H), 7.11(s, 2H), 6.68(d, 1H), 6.39(s, 2H), 4.84(dd, 2H), 3.81(s, 3H), 2.15(s, 3H); its IR(KBr, cm -1 ) data are: 3422, 3190, 31...

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Abstract

The invention discloses a novel ilaprazol M crystal form as well as a preparation method and an application thereof. The novel ilaprazol M crystal form disclosed by the invention is easy to prepare. The ilaprazol crystal form prepared by the preparation method disclosed by the invention is high in purity and low in impurity content. The preparation method needs less solvent, is low in production cost, simple to operate, gentle in reaction condition, easy to control, and good in repeatability, and can be used for stably obtaining a target product crystal form.

Description

technical field [0001] The invention relates to a new crystal form of ilaprazole and a preparation method thereof. Background technique [0002] Ilaprazole (Ilaprazole) chemical name: 2-[[(4-methoxy-3-methyl)-2-pyridyl]-methyl]sulfonyl]-5-(1 hydrogen-pyrrole-1 -base)-1 hydrogen-benzimidazole, its chemical structural formula is: [0003] [0004] Ilaprazole, also known as IY-81149, is a new type of irreversible proton pump inhibitor developed by Ilyang Pharmaceutical Company in Korea. Its inhibitory effect on Helicobacter pylori (HP) is stronger than that of omeprazole. It is 1 / 4 of omeprazole, less likely to produce drug resistance, and has no obvious toxic and side effects; compared with the original similar products, ilaprazole has overcome the delay in gastric emptying caused by the original similar products to varying degrees , parietal cell swelling and obvious rebound of gastric acid secretion after drug withdrawal, etc., and can enhance the curative effect on dys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/14A61P1/04A61P31/04
CPCC07B2200/13C07D401/14
Inventor 马攀勤丁厚锰王颖丽
Owner HARBIN SANLIAN PHARMA CO LTD
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