Preparation and Characterization of Two Crystalline Forms of 4-Amino-5-chloro-2-methoxy-N-[(2S, 4S)-1-ethyl-2-hydroxymethyl-4-pyrrolidinyl]benzamide (TKS159)

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For 4-amino-5-chloro-2-methoxy-N-[(2S, 4S)-1-ethyl-2-hydroxymethyl-4-pyrrolidinyl]benzamide (TKS159), two polymorphs, forms α and β, were prepared and characterized by means of X-ray powder diffractometry, thermal analysis, infrared spectroscopy and ^<13>C-NMR spectroscoy, both in the solution and solid phases. The X-ray powder diffraction analysis gave different patterns for forms α and β. In the thermogravimetry and differential thermal analysis profiles, form β exhibited characteristic endo- and exothermic peaks at 112.7℃ and 116.2℃, respectively, due to the partial melting-induced phase transition to form α without accompanying weight loss, and these were followed by an additional endothermic peak at 138.2℃ due to fusion. For form α, only an endothermic peak at 137.8℃ due to fusion was observed. The IR spectroscopic analyses of forms α and β gave different absorption bands assigned to N-H and O-H stretching, N-H bending, and C=O stretching vibrations. From the data obtained by thermal analysis, form α was shown to be thermodynamically more stable than form β.
2000-03-01