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Polymorphs

  • US 9,493,462 B2
  • Filed: 01/13/2016
  • Issued: 11/15/2016
  • Est. Priority Date: 05/04/2006
  • Status: Active Grant
First Claim
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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:

  • heating polymorph B or a mixture of polymorphs A and B to temperatures>

    40°

    C.;

    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

    ;

    and whereinsaid anhydrous polymorph B transforms reversibly into the polymorph A at temperature of 10-40°

    C., andsaid anhydrous polymorph B exhibits an X-ray powder diagram having characteristic reflections at the following d values;

    11.3 Å

    , 9.36 Å

    , 7.48 Å

    , 7.0 Å and

    3.77 Å

    .

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