eoc315 Mod.I crystalline compound and preparation method thereof
A compound and crystal form technology, applied in the application field of EOC315Mod.I crystal form in pharmaceuticals, can solve the problem of not finding the EOC315 crystal form, and achieve the effects of long tumor progression time, long survival time, and high response speed.
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Embodiment 1
[0066] Example 1 Preparation of EOC315Mod.I crystalline compound
[0067] The preparation of EOC315Mod.I type crystalline compound includes the following steps:
[0068] 1) 9g EOC315 base was dissolved in 90mL methanol to make EOC315 solution, 2.5g methanesulfonic acid was dissolved in 16mL methanol to make methanesulfonic acid solution;
[0069] 2) Begin at 50°C, add the methanesulfonic acid solution dropwise to the EOC315 solution, and continue heating for 15 minutes after dropping;
[0070] 3) The filtrate was distilled under reduced pressure, after steaming out part of the solvent, 200 ml of isopropanol was added to continue the distillation under reduced pressure until the feed liquid was about 250 mL, cooling and crystallization for 1 hour, suction filtration, and the filter cake was collected.
[0071] 4) Vacuum drying at 45°C to obtain EOC315Mod.I crystalline compound, the yield is 90.5-96.3%, and the purity is 99.1-99.9%.
[0072] Using X-ray diffraction analysis, ...
Embodiment 2
[0073] Example 2 Analysis of the EOC315Mod.I crystalline compound of Example 1 by differential scanning calorimetry (DSC)
[0074] The DSC trace was recorded in an aluminum pan at a heating rate of 10°C / min under a nitrogen atmosphere. It was measured that the EOC315 obtained in Example 1 had a sharp endothermic peak at 200.7°C, indicating that the EOC315 was a single Mod.I crystal form with a melting point of 200.7°C. The analysis results are as image 3 .
[0075] As is known to those of ordinary skill in the art, the melting temperature determined depends on the experimental conditions, especially the heating rate used. In addition, the melting temperature is affected by the purity of the substance. The reported melting temperatures were determined with a product that was at least 98.5% pure.
Embodiment 3
[0076] Example 3 Analysis of the EOC315Mod.I crystalline compound of Example 1 by X powder diffraction
[0077] X-ray powder diffraction data were recorded with germanium-induced monochromatic CuKα1-radiation at room temperature. At room temperature, 2θ scans were performed with an angular resolution of 0.08° between 3°≤2θ≤35° (step size 0.5°) using a small linear position-sensitive detector. X-ray powder diffraction pattern as figure 1 , where the 2θ and d(A) values are shown in Table 1.
[0078] One of ordinary skill in the art will appreciate that the obtained X-ray diffraction pattern may have measurement errors, which depend on the measurement conditions. In particular, it is generally known that the intensity of an X-ray diffraction pattern may fluctuate depending on the crystal habit of a substance and the measurement conditions used. In addition, the measurement error of the diffraction angle θ of a conventional X-ray diffraction pattern at a given temperature is...
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Abstract
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