Claims
- 1. Pioglitazone hydrochloride in Form II.
- 2. Pioglitazone hydrochloride in Form II having x-ray diffraction peaks at values of two theta of about 9.2, 10.4, 15.2, 16.4, 18.6, and 21.4.
- 3. The Form II pioglitazone hydrochloride of claim 2 exhibiting a DSC thermogram that has an endothermic peak at about 180° C. at a heating rate of 10° C. per minute.
- 4. A method for making pioglitazone hydrochloride in Form II comprising the steps of
a) dissolving pioglitazone hydrochloride in a solubilizing solvent to form a solution, b) adding water to the solution, c) collecting precipitated product.
- 5. The method of claim 4 further comprising the step of drying the product.
- 6. The method of claim 4 wherein the solubilizing solvent is selected from the group consisting of dimethylformamide, N,N-dimethylacetamide, acetic acid, methanol, and ethylene glycol.
- 7. The method of claim 4 further comprising the step, following step b), of cooling the mixture from step b).
- 8. The method of claim 4 wherein the dissolving is at an elevated temperature that is between room temperature and the water is added at the elevated temperature.
- 9. The method of claim 4 wherein the dissolving is at an elevated temperature that is between about 35° C. and about 70° C.
- 10. The method of claim 9 wherein the cooling is effected in two steps; first, from the elevated temperature to room temperature, and second, from room temperature to about 4° C.
- 11. The method of claim 4 further comprising the steps of:
e) suspending the product from step c) in a suspending solvent selected from the group consisting of acetone, methanol, ethanol containing up to about 5% water, methyl t-butyl ether, chloroform, dichloromethane, ethyl acetate, methyl ethyl ketone, iso-propyl alcohol, and butyl acetate, f) collecting pioglitazone hydrochloride Form II from the suspension, and
- 12. The method of claim 11 further comprising the step of drying the product collected.
- 13. A method of making pioglitazone hydrochloride in Form II comprising the steps of:
a) dissolving pioglitazone hydrochloride in a solubilizing solvent selected from the group consisting of dimethylformamide, N,N-dimethylacetamide, acetic acid, dimethyl sulfoxide, methanol, and ethylene glycol to form a solution, b) adding water to the solution, c) cooling the combination of solution and water to obtain a suspension, d) collecting pioglitazone hydrochloride Form II from the suspension.
- 14. The method of claim 13 further comprising the step of drying the collected product.
- 15. The method of claim 13 wherein the dissolving is at an elevated temperature between about room temperature and about 70° C.
- 16. The method of claim 13 wherein the dissolving is at a temperature between about 35° C. and about 70° C.
- 17. The method of claim 16 wherein the cooling is effected in two steps; first, from the elevated temperature to room temperature, and second, from room temperature to about 4° C.
- 18. A method for making pioglitazone hydrochloride in Form II comprising the steps of combining pioglitazone hydrochloride in Form I in water to form a slurry and collecting pioglitazone hydrochloride Form II from the slurry.
- 19. A method for making pioglitazone hydrochloride in Form I comprising the steps of:
dissolving pioglitazone hydrochloride in a solubilizing solvent selected from dimethyl formamide, dimethyl acetamide, acetic acid, methanol, and ethylene glycol at a temperature between about 26° C. and 65° C. to form a solution, cooling the solution whereby a precipitate forms, and collecting pioglitazone hydrochloride Form I.
- 20. The method for claim 19 wherein the pioglitazone hydrochloride is dissolved at a temperature greater than about 35° C.
- 21. The method of claim 20 wherein the pioglitazone hydrochloride is dissolved at a temperature between about 60° C. and 65° C.
- 22. The method of claim 20 wherein the cooling is effected in two steps: first to room temperature, and second, to about 4° C.
- 23. A method for making pioglitazone hydrochloride in Form I comprising the steps of:
a) dissolving pioglitazone hydrochloride in a solubilizing solvent selected from dimethyl formamide and dimethyl sulfoxide at a temperature between about 26° C. and 65° C. to form a solution, b) adding to the solution an anti-solvent, c) cooling the mixture of solution and anti-solvent whereby a precipitate forms, and d) collecting pioglitazone hydrochloride Form I.
- 24. The method of claim 20 wherein the anti-solvent is selected from the group consisting of ethyl acetate, methyl ethyl ketone, absolute ethanol, and acetone.
- 25. The method of claim 20 wherein the cooling is effected in two steps: first to room temperature, and second, to about 4° C.
RELATED APPLICATIONS
[0001] The present application claims the benefit of the filing date of U.S. Provisional Patent Application Serial No. 60/326,112, filed Sep. 28, 2001.
Provisional Applications (1)
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Number |
Date |
Country |
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60326112 |
Sep 2001 |
US |