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Preparation method for eutectic hydrate crystal form II of AHU-377 and diovan trisodium salt

  • US 10,442,775 B2
  • Filed: 11/10/2016
  • Issued: 10/15/2019
  • Est. Priority Date: 12/08/2015
  • Status: Active Grant
First Claim
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1. A preparation method of trisodium AHU-377 and Valsartan co-crystal hydrate Form II, wherein the X-ray powder diffraction pattern (CuKα

  • radiation) of said Form II has characteristic peaks at 2theta values of 4.3°

    ±

    0.2°

    , 5.0°

    ±

    0.2° and

    12.8°

    ±

    0.2°

    , said preparation method comprises the following steps;

    Step 1;

    preparing a clear solution containing trisodium AHU-377 and Valsartan, wherein said clear solution comprises a first solvent and a second solvent;

    the first solvent is an anti-solvent of Form II, and can form azeotrope with water, the second solvent is a good solvent of Form II, and the boiling point of the second solvent is lower than that of the first solvent;

    Step 2;

    evaporating the clear solution obtained in Step 1 under vacuum or under nitrogen purging to remove the second solvent and water from the system; and

    Step 3;

    mixing the system obtained in Step 2 with water, a third solvent and with or without seed crystals of Form II, then stirring for crystallization, filtering, washing and drying to obtain Form II, wherein said third solvent is an anti-solvent of Form II, which is miscible in the first solvent, and water is soluble in said third solvent.

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