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Claims for Patent: 6,777,423

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Claims for Patent: 6,777,423

Title: Crystalline tiotropium bromide monohydrate, processes for the preparation thereof, and pharmaceutical compositions
Abstract:Crystalline monohydrate of (1.alpha.,2.beta.,4.beta.,5.alpha.,7.beta.)-7-[(hydroxydi-2-thienylacetyl) oxy]-9,9-dimethyl-3-oxa-9-azoniatricyclo[3.3.1.0.sup.2,4 ]nonane bromide (tiotropium bromide monohydrate), processes for the preparation thereof, pharmaceutical compositions thereof, and their use.
Inventor(s): Banholzer; Rolf (Stuttgart, DE), Sieger; Peter (Mittelbiberach, DE), Kulinna; Christian (Mainz, DE), Trunk; Michael (Ingelheim, DE), Graulich; Manfred (Waldalgesheim, DE), Specht; Peter (Ober-Hilbersheim, DE), Meissner; Helmut (Ingelheim, DE), Mathes; Andreas (Ockenheim, DE)
Assignee: Boehringer Ingelheim Pharma KG (Ingelheim, DE)
Application Number:10/354,521
Patent Claims: 1. Crystalline tiotropium bromide monohydrate having an endothermic peak at 230.degree. C..+-.5.degree. C. occurring during thermal analysis using DSC at a heating rate of 10 K/min.

2. Crystalline tiotropium bromide monohydrate having an IR spectrum comprising bands at wave numbers 3570, 3410, 3105, 1730, 1260, 1035, and 720 cm.sup.-1.

3. Crystalline tiotropium bromide monohydrate according to claim 1, having an IR spectrum comprising bands at wave numbers 3570, 3410, 3105, 1730, 1260, 1035, and 720 cm.sup.-1.

4. Crystalline tiotropium bromide monohydrate according to claim 1, having a single monoclinic cell having the following dimensions: a=18.0774 .ANG., b=11.9711 .ANG., c=9.9321 .ANG., .beta.=102.691.degree., and V=2096.96 .ANG..sup.3.

5. Crystalline tiotropium bromide monohydrate according to claim 2, having a single monoclinic cell having the following dimensions: a=18.0774 .ANG., b=11.9711 .ANG., c=9.9321 .ANG., .beta.=102.691.degree., and V=2096.96 .ANG..sup.3.

6. Crystalline tiotropium bromide monohydrate according to claim 3, having a single monoclinic cell having the following dimensions: a=18.0774 .ANG., b=11.9711 .ANG., c=9.9321 .ANG., .beta.=102.6910.degree., and V=2096.96 .ANG..sup.3.

7. A process for preparing crystalline tiotropium bromide monohydrate according to claim 1, the process comprising: (a) dissolving tiotropium bromide in water to obtain a solution; (b) heating the resulting solution; (c) adding activated charcoal to the heated solution; (d) removing the activated charcoal; and (e) allowing the solution to slowly cool to obtain crystalline tiotropium bromide monohydrate.

8. A process for preparing crystalline tiotropium bromide monohydrate according to claim 1, the process comprising: (a) dissolving tiotropium bromide in water to obtain a solution; (b) heating the resulting solution to more than 50.degree. C.; (c) adding activated charcoal to the heated solution; (d) removing the activated charcoal; and (e) allowing the solution to slowly cool to obtain crystalline tiotropium bromide monohydrate.

9. The process according to claim 8, wherein 0.4 to 1.5 kg of water are used per mole of tiotropium bromide in step (a).

10. The process according to claim 9, wherein 10 g to 50 g of activated charcoal per mole of tiotropium bromide is added in step (c).

11. The process according to claim 10, wherein the activated charcoal added in step (c) is stirred for between 5 and 60 minutes before it is removed in step (d).

12. The process according to claim 11, wherein step (d) is performed by filtration of the solution.

13. The process according to claim 12, wherein the solution of step (e) is cooled to a temperature of 20.degree. C.-25.degree. C. at a cooling rate of 1 to 10.degree. C. per 10 to 30 minutes.

14. A process for preparing the crystalline tiotropium bromide monohydrate according to claim 1, the process comprising: (a) dissolving tiotropium bromide in water to obtain a solution; (b) heating the resulting solution; and (c) allowing the solution to slowly cool to obtain crystalline tiotropium bromide monohydrate.

15. A process for preparing crystalline tiotropium bromide monohydrate according to claim 1, the process comprising: (a) dissolving tiotropium bromide in water to obtain a solution; (b) heating the solution of step (a); (c) adding activated charcoal to the heated solution of step (b); (d) removing the activated charcoal from the solution of step (c); and (e) allowing the solution to slowly cool to obtain crystalline tiotropium bromide monohydrate.

16. The process of claim 15, wherein the solution of step (a) is heated to more than 50.degree. C.
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