Polymorphs
First Claim
Patent Images
1. A method of preparing an anhydrous polymorph A of the compound 1-[(4-methyl-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-(R)-amino-piperidin-1-yl)-xanthine, the method comprising:
- (a) dissolving 1-[(4-methyl-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-(R)-amino-piperidin-1-yl)-xanthine in absolute ethanol to provide a solution;
(b) refluxing the solution to provide a hot solution and, optionally filtering the hot solution to provide a hot filtrate,(c) cooling the hot solution or the hot filtrate until crystallisation sets in,(d) diluting the cooled solution or the cooled filtrate with a solvent to provide a solvent mixture,(e) suction filtering the solvent mixture, and(f) drying the solids collected by filtration at 45°
C. in vacuo to provide said anhydrous polymorph A;
whereinsaid anhydrous polymorph A melts at 206±
3°
C., andsaid anhydrous polymorph A exhibits an X-ray powder diagram having characteristic reflections at the following d values;
11.59 Å
, 7.60 Å
, 7.15 Å
, 3.86 Å
, 3.54 Å and
3.47 Å
.
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Abstract
The invention relates to polymorphous crystal modifications of a DPP-IV inhibitor, the preparation thereof and the use thereof for preparing a medicament.
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Citations
12 Claims
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1. A method of preparing an anhydrous polymorph A of the compound 1-[(4-methyl-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-(R)-amino-piperidin-1-yl)-xanthine, the method comprising:
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(a) dissolving 1-[(4-methyl-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-(R)-amino-piperidin-1-yl)-xanthine in absolute ethanol to provide a solution; (b) refluxing the solution to provide a hot solution and, optionally filtering the hot solution to provide a hot filtrate, (c) cooling the hot solution or the hot filtrate until crystallisation sets in, (d) diluting the cooled solution or the cooled filtrate with a solvent to provide a solvent mixture, (e) suction filtering the solvent mixture, and (f) drying the solids collected by filtration at 45°
C. in vacuo to provide said anhydrous polymorph A;
whereinsaid anhydrous polymorph A melts at 206±
3°
C., andsaid anhydrous polymorph A exhibits an X-ray powder diagram having characteristic reflections at the following d values;
11.59 Å
, 7.60 Å
, 7.15 Å
, 3.86 Å
, 3.54 Å and
3.47 Å
. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12)
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Specification