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Crystalline anti-cholinergic tiotropium crystal

A technology of tiotropium bromide and crystals, which is applied in the field of crystalline anticholinergic drug tiotropium bromide crystals, and can solve problems such as not giving test results

Active Publication Date: 2006-08-23
CHIA TAI TIANQING PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is as follows: take tiotropium bromide monohydrate as the starting material, carefully dry under reduced pressure at above 50°C, preferably 60-100°C or store it on a suitable desiccant for 12-96 hours to obtain crystalline Tiotropium bromide water, crystal unit lattice parameters are respectively a=10.4336 (2) , b=11.3297 (3) , c=17.6332 (4) , α=90 °, β=105.158 (2) °, γ=90°, X-ray powder diffraction analysis data of anhydrous tiotropium bromide crystalline structure are listed in the patent, but no infrared, DSC and other test results are given

Method used

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  • Crystalline anti-cholinergic tiotropium crystal
  • Crystalline anti-cholinergic tiotropium crystal
  • Crystalline anti-cholinergic tiotropium crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 30g of tiotropium bromide crude product (light yellow), put it in a 500ml three-neck glass bottle, add 300ml of acetone-methanol-water (30:30:2), stir and heat up to 50°C, dissolve the solid, filter, and cool the filtrate to - Crystallize at 10-5°C for 24 hours, precipitate colorless crystals, filter, wash with acetone, and place at room temperature for 8 hours to obtain 21.5 g of white crystals, yield 71.7%, melting point (decomposition): 218-220°C, obtained by Fischer The moisture measured by the method is 0.20%. The purity measured by high performance liquid chromatography is 99.6% (normalized method)

Embodiment 2

[0031] Take 15g of tiotropium bromide crude product (light yellow), put it in a 500ml three-necked glass bottle, add 230ml of acetone-methanol-water (30:30:1), stir and heat up to reflux, dissolve the solid, filter, and concentrate the filtrate to about 50ml , the filtrate was cooled to -10-5°C to allow crystallization for 24 hours, filtered, washed with acetone, and dried under reduced pressure at 50°C to obtain 13.4 g of white crystals, the measured water content was 0.41%, and the yield was 89.3%. Melting point (decomposition): 218~219℃.

Embodiment 3

[0033] Take 16g of tiotropium bromide monohydrate, put it in a 500ml three-neck glass bottle, add 130ml of acetone-methanol-water (30:30:1), stir and heat up to reflux, dissolve the solid, filter, and cool the filtrate to -10~5 Crystallize at ℃ for 24 hours, and colorless crystals are precipitated, filtered, washed with acetone, and left at room temperature for 8 hours to obtain 12.5 g of white crystals, with a yield of 81.1%. was 0.24%.

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Abstract

The invention relates to crystal unhydrous (1R,2R,4S,5S,7S)-7-[2-hydroxy-2,2-bis(2-thienyl) acetoxy]-9,9-dimethyl-3-oxa-9-azo cation tricyclo octane [3.3.1.02.4] nonane bromide, clinic use of tiotropium bromide anhydrous crystal as anti-cholinergic medicines, and preparation process of tiotropium bromide anhydrous crystal.

Description

technical field [0001] The present invention relates to crystalline anhydrous (1R, 2R, 4S, 5S, 7S)-7-[2-hydroxy-2,2-bis(2-thienyl)acetoxy]-9,9-dimethyl- 3-Oxa-9-azation tricyclooctane [3.3.1.0 2.4 ] Nonane bromide crystal, common name Tiotropium bromide (Tiotropium Bromide), its preparation method and pharmaceutical composition, can be used as anticholinergic drug, be used for treating asthma and COPD (chronic obstructive pulmonary disease) clinically. Its chemical structural formula is as follows: [0002] Background technique [0003] The crystalline anhydrous (1R, 2R, 4S, 5S, 7S)-7-[2-hydroxy- 2,2-bis(2-thienyl)acetoxy]-9,9-dimethyl-3-oxa-9-azacation tricyclooctane [3.3.1.0 2.4 ] The preparation method of nonane bromide crystal. The method is as follows: take tiotropium bromide monohydrate as the starting material, carefully dry under reduced pressure at above 50°C, preferably 60-100°C or store it on a suitable desiccant for 12-96 hours to obtain crystalline Tiotr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/18A61K31/439A61P11/06A61P11/00C07D221/00C07D209/00C07D303/00
Inventor 张爱明高勇
Owner CHIA TAI TIANQING PHARMA GRP CO LTD
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