Crystal forms of LY334370 HCl: isolation, solid-state characterization, and physicochemical properties

J Pharm Sci. 2003 Jun;92(6):1196-205. doi: 10.1002/jps.10373.

Abstract

LY334370 HCl, a 5HT1f agonist investigated for the treatment of migraines, was identified in five crystal forms: three anhydrates (I-III), a dihydrate, and an acetic acid solvate. The identification and characterization of these crystal forms by optical microscopy, differential scanning calorimetry, thermogravimetric and moisture sorption analyses, solid-state NMR spectroscopy, and X-ray crystallography (Form I only) are presented. Physical properties, including hygroscopicity, solubility, and intrinsic dissolution rate, were assessed for Form I and the dihydrate, the two most viable crystal forms for commercial development. Surprisingly, anhydrous Form I was found to be the thermodynamically most stable crystal form in water, dissolving six times slower than the dihydrate, a difference that correlates well with the rank order of aqueous solubility.

Publication types

  • Comparative Study

MeSH terms

  • Benzamides / chemistry*
  • Benzamides / isolation & purification*
  • Chemical Phenomena
  • Chemistry, Physical
  • Crystallization
  • Crystallography, X-Ray
  • Drug Stability
  • Humidity
  • Indoles / chemistry*
  • Indoles / isolation & purification*
  • Magnetic Resonance Spectroscopy
  • Molecular Structure
  • Powders
  • Serotonin Receptor Agonists / chemistry*
  • Serotonin Receptor Agonists / isolation & purification*
  • Solubility
  • Solvents / chemistry
  • Time Factors

Substances

  • 4-fluoro-N-(3-(1-methyl-4-piperidinyl)-1H-indol-5-yl)benzamide
  • Benzamides
  • Indoles
  • Powders
  • Serotonin Receptor Agonists
  • Solvents