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A Crystalline form of 4-(4-amino-3-fluorophenoxy)-N-methylpyridine-2- carboxamide

IP.com Disclosure Number: IPCOM000233812D
Publication Date: 2013-Dec-23
Document File: 2 page(s) / 74K

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A Crystalline form of 4-(4-amino-3-fluorophenoxy)-N-methylpyridine-2- carboxamide

4-(4-amino-3-fluorophenoxy)-N-methylpyridine-2-carboxamide referred to as Compound I, has the following formula:

Compound I

Crude Compound I can be prepared according to processes that are known in art, for example, according to the process described in US 2013/0116442, Method 2a, pag. 5. Alternatively, crude Compound I can be prepared according to a process relating to des-fluoro analogues of Compound I, as described in D. Bankston et al., Org. Proc. Res. Dev. 2002, 6, 777. The obtained crude material was isolated from water upon pH adjustment to 9.5 with aqueous ammonia to obtain a crystalline form of Compound I.

    The samples of Compound I were analyzed by X-ray powder diffraction ("XRPD"). Figure 1 presents the XRPD of the obtained crystalline form.

Figure 1:An XRPD pattern of a crystalline form of Compound I


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    According to Figure 1, the crystalline form of Compound I may be characterized by XRPD peaks at 8.2, 12.1, 12.5, 15.9, 16.5, 16.7, 18.6, 18.9, 20.1,


22.8, 23.2, 23.7, 24.3, 25.2, 28.1, 28.4 and 34.1 °2θ ± 0.2 °2θ.

XRPD method

    Samples after being powdered in a mortar and pestle are applied directly on silicon plate holder. The X-ray powder diffraction pattern was measured with Philips X'Pert PRO X-ray powder diffractometer, equipped with Cu irradiation source =1.54184 Ǻ (Ǻngström), X'Celerator (2.022º 2 Ө) detector. Scanning parameters: angle range: 3-...