EOC 315 Mod. I crystal form compound and its preparation method
A technology of compound and crystal form, which is applied in the field of pharmaceutical application of EOC315Mod.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0066] The preparation of embodiment 1EOC315Mod.I crystal form compound
[0067] The preparation of EOC315Mod.I type crystal compound comprises the following steps:
[0068] 1) Dissolve 9g EOC315 alkali in 90mL methanol to make EOC315 solution, and dissolve 2.5g methanesulfonic acid in 16mL methanol to make methanesulfonic acid solution;
[0069] 2) Start at 50°C, add the methanesulfonic acid solution dropwise into the EOC315 solution, and continue heating for 15 minutes after the drop is complete;
[0070] 3) Distill the filtrate under reduced pressure, evaporate part of the solvent, add 200ml of isopropanol and continue the distillation under reduced pressure until the feed liquid is about 250mL, cool down and crystallize for 1 hour, filter with suction, and collect the filter cake.
[0071] 4) EOC315Mod.I crystal compound was obtained by vacuum drying at 45°C, with a yield of 90.5-96.3% and a purity of 99.1-99.9%.
[0072] Using X-ray diffraction analysis, the figure 1 ...
Embodiment 2
[0073] Example 2 Analysis of the EOC315Mod.I crystal form compound of Example 1 by differential scanning calorimetry (DSC)
[0074] In a nitrogen atmosphere, the DSC trace was recorded on an aluminum plate at a heating rate of 10°C / min. It was measured that EOC315 obtained in Example 1 had a sharp endothermic peak at 200.7°C, indicating that EOC315 was a single Mod.I crystal form with a melting point of 200.7°C. Analytical results such as image 3 .
[0075] Those of ordinary skill in the art know that the measured melting temperature depends on the experimental conditions, especially the heating rate used. Additionally, the melting temperature is affected by the purity of the substance. Reported melting temperatures were determined on products with a purity of at least 98.5%.
Embodiment 3
[0076] Example 3 Analysis of the EOC315Mod.I Crystal Form Compound of Example 1 by X Powder Diffraction
[0077] X-ray powder diffraction data were recorded with germanium-induced monochromatization 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 2θ and d(A) values are shown in Table 1.
[0078] Those of ordinary skill in the art will appreciate that the obtained X-ray diffraction patterns may have measurement errors, which errors 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 te...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More