Crystalline form of Adefovir dipivoxil and preparing process thereof

Crystalline form of Adefovir dipivoxil and preparing process thereof

  • CN 1,435,420 A
  • Filed: 11/19/2002
  • Published: 08/13/2003
  • Est. Priority Date: 11/19/2002
  • Status: Active Application
First Claim
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1. , a kind of adefovir dipivoxil novel crystal habit and preparation method thereof, it is characterized in that adefovir ester that crystallization in the crystallization solvent is gone out, again be dissolved in the organic solvent, evaporated under reduced pressure solvent again, it comprises that crystallization goes out adefovir ester from the solution that contains 6-45% adefovir ester and about 55-94% crystallization solvent, again be dissolved in it in organic solvent again, get colourless well-illuminated solution, in 30-60 ℃

  • of solvent evaporated in vacuo, obtain oily matter, be cooled to 30 ℃

    gradually, be cured as white solid, grind, 60 ℃

    of vacuum-drying 8 hours, the adefovir ester of white powder novel solid crystal habit, use Cu-Ka radiation (λ

    =1.5405 ), as follows to spend the X-ray powder diffraction spectral signature that 2 θ

    represent.2 θ

    spacings (d value) I/I 03.68????????????????23.99???????????????????1007.36????????????????12.00???????????????????257.84????????????????11.27???????????????????4910.12???????????????8.73????????????????????812.36???????????????7.16????????????????????1114.80???????????????5.98????????????????????915.16???????????????5.84????????????????????2016.36???????????????5.41????????????????????1417.28???????????????5.13????????????????????3118.04???????????????4.91????????????????????2520.16???????????????4.40????????????????????1420.44???????????????4.34????????????????????921.28???????????????4.17????????????????????1122.28???????????????3.99????????????????????2726.08 3.41 10 novel crystalline form attitudes, its feature are that also its DSC (dsc) endothermic transition is at about 95 ℃

    .

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