Polymorphs
First Claim
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1. A method of preparing polymorph C 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) refluxing a solution of 1-[(4-methyl-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-(R)-amino-piperidin-1-yl)-xanthine in methanol to provide a hot methanolic solution,(b) cooling the hot methanolic solution to a temperature of 40-60°
C. to provide a cooled methanolic solution,(c) adding tert-butylmethylether to the cooled methanolic solution to form a suspension,(d) cooling the suspension first to a temperature of 15-25°
C. and then to a temperature of 0-5°
C. to provide crystals,(e) suction filtering the crystals, and(f) drying the crystals obtained in step (e) in vacuo at a temperature of 70°
C. to provide Polymorph C,wherein Polymorph C loses water at a temperature of 30-100°
C. and exhibits further thermal effects at a temperature of about 150°
C. and about 175°
C. in a differential scanning calorimetry (DSC) analysis.
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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
3 Claims
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1. A method of preparing polymorph C 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) refluxing a solution of 1-[(4-methyl-quinazolin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-(3-(R)-amino-piperidin-1-yl)-xanthine in methanol to provide a hot methanolic solution, (b) cooling the hot methanolic solution to a temperature of 40-60°
C. to provide a cooled methanolic solution,(c) adding tert-butylmethylether to the cooled methanolic solution to form a suspension, (d) cooling the suspension first to a temperature of 15-25°
C. and then to a temperature of 0-5°
C. to provide crystals,(e) suction filtering the crystals, and (f) drying the crystals obtained in step (e) in vacuo at a temperature of 70°
C. to provide Polymorph C,wherein Polymorph C loses water at a temperature of 30-100°
C. and exhibits further thermal effects at a temperature of about 150°
C. and about 175°
C. in a differential scanning calorimetry (DSC) analysis. - View Dependent Claims (2, 3)
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Specification