Crystalline forms of dmxaa sodium salt
A technology of sodium salt and crystal form, applied in organic chemistry, antineoplastic drugs, drug combination, etc., can solve problems such as difficult to obtain uniformity and change
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[0257] Abbreviations appearing in the examples and other parts have the following meanings:
[0258]
[0259]
[0260] experiment:
[0261] X-ray Powder Diffraction (PXRD): PXRD uses CuK α Ray (K α1 with K α2 The ratio is 2:1) on a Philips 1710 X-ray powder diffractometer. X-ray powder diffraction measurements are done in reflectance mode. Interplanar spacing d at wavelength Calculated from the 2θ values below. Usually the error of the 2θ value is ±0.1 to ±0.2°. Therefore, the experimental error of the interplanar spacing depends on the peak position.
[0262] Raman spectrum: The Fourier transform Raman spectrum generated when the sample was irradiated by a near-infrared Nd:YAG laser at 1064 nm was recorded in a Bruker RFS 100 Fourier transform Raman system, and detected with a germanium detector cooled by liquid nitrogen. Each sample with a resolution of 2cm -1 64 scans were accumulated and a laser power of 100 mW was typically applied.
[0263] DSC: Differ...
Embodiment A1
[0280] 897 mg of the DMXAA sodium salt methanolate form M of Reference Example was dissolved in 4.0 mL of water at room temperature. The solution was filtered through a 0.2 μm Millipore filter device into a 250 mL round bottom flask where the solution was frozen at -78°C with solid carbon dioxide (dry ice). Thereafter, it was freeze-dried using a Christ Beta 2-8, L9-2 type freeze dryer under the conditions of a pressure of 0.090 mbar and a freezing temperature of -89°C. After freeze-drying for 18 hours, the resulting dry powder was subjected to X-ray powder diffraction and Raman spectroscopy. The X-ray powder diffraction pattern has a single characteristic peak at 2θ=25.7°, which is a typical mesomorph or amorphous, and is called crystal form A (or mesomorph A). The X-ray powder diffraction pattern of crystal form A is as follows figure 2 shown.
[0281] Stability: Mesogen Form A is ambient stable for at least 2 months when stored in a sealed container under nitrogen.
[...
Embodiment B1
[0284] Example B 1: Preparation of Form B from Mesomorph Form A
[0285] About 50 mg of DMXAA sodium salt mesomorph form A in Example A1 was stored at 40° C. in a humidity chamber at a relative humidity of 75% (corresponding to a water activity of 0.75) for about 5 days. Unexpectedly, the X-ray powder diffraction pattern of this sample shows that what is obtained is a new crystal form, and its X-ray powder diffraction pattern is as follows image 3 As shown, its peak position is shown in Table 2 below. The Raman spectrum of crystal form B is as Figure 14 shown.
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