×

Polymorphs

  • US 9,266,888 B2
  • Filed: 08/19/2014
  • Issued: 02/23/2016
  • Est. Priority Date: 05/04/2006
  • Status: Active Grant
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±



    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 all claims
  • 0 Assignments
Timeline View
Assignment View
    ×
    ×