A new crystal of ticagrelor and its preparation method
A ticagrelor and crystallization technology, which is applied in the field of ticagrelor new crystallization and its preparation, can solve the problems of high toxicity of chloroform as a crystallization solvent, unsuitable for large-scale production, uneven crystal particles, and the like, and saves the preparation preparation process. , excellent stability, simple preparation method
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Embodiment 1
[0064] Embodiment 1: Preparation of ticagrelor crystals
[0065] Add 10g of crude ticagrelor (reference Bioorganic & Medicinal Chemistry Letters 22 (2012) 3598~3602, purity 98%) and 80mL ethyl acetate into the reaction flask, heat to 55±5°C, stir to dissolve, keep at the same temperature , add 40mL of n-hexane dropwise, solid precipitates out, keep stirring at the same temperature for 2h, then cool down to 15~30°C, continue stirring for 1h, filter and dry to obtain 9.1g of white crystalline solid with HPLC purity of 99.6%. Small crystalline particles, fluffy appearance, low viscosity. Get the obtained crystalline sample and carry out XRD detection, the results are shown in Table 1, and the spectrum is shown in the attached figure 1 . In addition, the obtained crystallization samples were taken for particle size detection, the results are shown in Table 2, and the spectrograms are shown in the attached figure 2 .
[0066] Table 1 Example 1 obtained ticagrelor crystalline p...
Embodiment 2~5
[0071] Embodiment 2~5: Preparation of ticagrelor crystals
[0072] Referring to the preparation method of Example 1, the crystallization conditions were changed, and the experimental results are shown in Table 3.
[0073] Table 3 Embodiment 2~5 experimental results
[0074] .
[0075] Table 4 The characteristic peak data of ticagrelor crystal powder X-ray diffraction obtained in Example 2-5
[0076] .
[0077] It can be seen from the experimental results in Table 2 that all the preparation methods of the present invention can obtain the new crystals of ticagrelor of the present invention.
Embodiment 6
[0078] Embodiment 6: Preparation of ticagrelor crystals
[0079] Add 10g of crude ticagrelor (reference Bioorganic & Medicinal Chemistry Letters 22 (2012) 3598~3602, purity 98%) and 60mL ethyl acetate into the reaction flask, heat to 55±5°C, stir to dissolve, add dropwise quickly ( Add 60mL of n-hexane below 25℃ at a drop rate of about 10mL / min, quickly cool down in an ice bath to 15~30℃ (about 5~10min), stir for 4h, filter, and dry to obtain ticagrelor crystals 9.4g, HPLC purity 99.6%. Get the obtained crystallization sample and carry out XRD detection, the results are shown in Table 3, and the obtained collection of patterns is shown in the attached image 3 . In addition, the obtained crystallization sample is taken for particle size detection, and the results are shown in Table 6, and the obtained collection of illustrative plates is shown in the attached Figure 4 .
[0080] Table 5 The characteristic peak data of ticagrelor crystal powder X-ray diffraction obtained i...
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