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Bilastine crystal form and preparation method thereof

A crystal form and drug technology, applied in the field of drug preparation, can solve problems such as undisclosed crystal form information

Inactive Publication Date: 2014-05-14
北京博泽德润医药科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent US5877187 only involves the bilastine production method, and does not disclose relevant crystal form information

Method used

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  • Bilastine crystal form and preparation method thereof
  • Bilastine crystal form and preparation method thereof
  • Bilastine crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put an appropriate amount of bilastine into 100 times the volume of isopropanol, and heat to reflux for about 15-20 minutes while stirring under a nitrogen atmosphere. Cool slowly, and cool the reaction liquid to about 50°C over 6 hours, and stop stirring. Cool the reaction solution to room temperature, stir again for 3 hours, filter, wash the solid with a small amount of cold isopropanol, and dry it in vacuum at 35-40°C to constant weight to obtain a stable crystal form of bilastine, the obtained bilastine X-ray powder diffraction 2θ (±0.2) data are: 11.30, 12.50, 17.18, 18.94, 19.80, 21.14, 22.68, 24.92.

[0019]

Embodiment 2

[0021] Put 830g of bilastine crude product and 83L of isopropanol into a 100L reactor, protect it with nitrogen, heat to reflux, dissolve and clarify, filter out the insoluble matter while it is hot, cool the filtrate to room temperature, stir and crystallize for 10-12h, and filter with suction. The filter cake was washed with a small amount of isopropanol, dried in vacuum at 50-60°C to constant weight, about 45-50h, and 610-660g of white solid was obtained, and a stable crystal form of bilastine was obtained, and the obtained bilastine X- X-ray powder diffraction 2θ (±0.2) data are: 11.30, 12.50, 17.18, 18.94, 19.80, 21.14, 22.68, 24.92.

Embodiment 3

[0023] Put an appropriate amount of bilastine into 100 times the volume of methanol ethyl acetate (1:1 mixture), and heat to reflux for about 15-20 minutes while stirring under a nitrogen atmosphere. Cool slowly, and cool the reaction liquid to about 50°C over 6 hours, and stop stirring. The reaction solution was cooled to room temperature, stirred again for 3 hours, filtered, washed with a small amount of cold ethyl acetate, dried in vacuum at 35-40°C to constant weight, and the yield was calculated.

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Abstract

The invention relates to preparation of a medicine, and particularly relates to a crystal form of 2[4-(2-{4-[1-(2-ethoxyethyl)-1H-benzimidazole-2-yl]-piperidine-1-yl}-ethyl)-phenyl]-2-methyl propionic acid and a preparation method. The invention provides a stable bilastine crystal form and a preparation technology scheme thereof. The X-ray powder diffraction 2 theta (+ / -0.2) data of the stable bilastine crystal form are 11.30, 12.50, 17.18, 18.94, 19.80, 21.14, 22.68 and 24.92.

Description

technical field [0001] The present invention relates to a preparation of medicine, in particular to a 2-[4-(2-{4-[1-(2-ethoxyethyl)-1H-benzimidazol-2-yl]- Crystal form of piperidin-1-yl}-ethyl)-phenyl]-2-methylpropionic acid and its preparation method. Background technique [0002] Bilastine (CAS No. 202189-78-4), 2-[4-(2-{4-[1-(2-ethoxyethyl)-1H-benzimidazol-2-yl ]-piperidin-1-yl}-ethyl)-phenyl]-2-methylpropionic acid is the second-generation histamine H1 receptor antagonist developed by Spain's FAES Pharmaceutical Company, which was approved for marketing in the European Union in 2010 . [0003] Bilastine (CAS No. 202189-78-4), 2-[4-(2-{4-[1-(2-ethoxyethyl)-1H-benzimidazol-2-yl ]-piperidin-1-yl}-ethyl)-phenyl]-2-methylpropionic acid is the second-generation histamine H1 receptor antagonist developed by Spain's FAES Pharmaceutical Company, which was approved for marketing in the European Union in 2010 . [0004] The crystal form of a drug is directly related to its so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
CPCY02P20/55C07D401/04
Inventor 张荣立程璇宋春光王洪新
Owner 北京博泽德润医药科技开发有限公司
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