Palbociclib polycrystal form and preparation method thereof

Abstract

The invention relates to a palbociclib polycrystal form and a preparation method thereof. In an X-ray powder diffraction pattern, characteristic peaks exist near the angles 2theta of 7.17 degrees, 7.62 degrees, 7.82 degrees, 8.49 degrees, 11.62 degrees, 11.81 degrees, 12.62 degrees, 22.96 degrees, 25.10 degrees and 25.63 degrees, wherein 2theta can have the deviation of + / - 0.2 degree; a differential scanning calorimetry analysis chart shows that an exothermic peak appears near the temperature of 207 DEG C. The preparation method of the crystal form C is easy to implement, a solvent is small in dosage and free of toxicity, the production cost is low, and the preparation method has obvious advantages in the aspect of industrialization; a substantial progress of the whole novel crystal form preparation process is achieved, and the process has significant progressiveness.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a polymorphic form of palbociclib and a preparation method thereof. Background technique [0002] Palbociclib, the chemical name is 6-acetyl-8-cyclopentyl-5-methyl-2-[[5-(piperazin-1-yl)pyridin-2-yl]amino]-8H- Pyrido[2,3-D]pyrimidin-7-one, the structural formula (I) is as follows: [0003] [0004] Developed by Pfizer, the drug is the first CDK4 / 6 inhibitor approved by the US FDA in February 2015 for late or metastatic ER in menopausal women. + / HER 2- Breast cancer, Palbociclib is a breakthrough, oral, targeted CDK4 / 6-specific inhibitor for the selective inhibition of cyclin-dependent kinases 4 and 6 (CDK4 / 6) , the first-line treatment for restoring cell cycle control and blocking tumor cell proliferation. The successful research of this new drug provides an important new option for patients with metastatic breast cancer, so it has broad market pros...

AI Technical Summary

Problems solved by technology

[0006] The X-ray diffraction spectrum of the Chinese patent CN 105085517A free base hydrate includes the following characteristic peaks indicated by the 2θ angles: 5.7°, 7.8°, 8.3°, 8.9°, 11.4°, 13.1° and 16.7°, the accuracy of the 2θ value It is ±0.2°, and its preparation process is precipitated from an aqueous solution rich in inorganic salts, which will bring the risk of excess residue on ignition. The prepared product has not been compared with the original research prescription for the dissolution rate of the preparation, so it cannot guarantee that it can meet the requirements of the pharmaceutical crystal form

[0007] In summary, there are not many crystalline forms of palbociclib reported in the literature at present, but the drug has significant curative effect and has a broad market prospect. Therefore, it is necessary to develop new pharmaceutical crystalline forms of palbociclib

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