Crystal form G of ibrutinib and preparation method

A technology of ibrutinib and its crystal form, which is applied in the field of medicinal chemistry, can solve problems such as difficulty in implementing industrialization of stirring, low absorption bioavailability, and poor control of the production process, achieving good controllability and reproducibility, The effect of high bioavailability and cheap solvent

Inactive Publication Date: 2016-06-08
孙霖
7 Cites 24 Cited by

AI-Extracted Technical Summary

Problems solved by technology

The operation of this method is cumbersome, there are repeated heating and cooling in the operation, and the production process is not easy to control
[0006] Suzhou Jingyun CN104327085A discloses another crystal form A (hereinafter referred to as crystal form A'), and its reported preparation method has three kinds: Method 1, dissolving the crude product of ibrutinib in a mixed solution of isopropanol and n-heptane In the method, crystal form A' was obtained by stirring at a speed of 750 revolutions per minute at room temperature. It is very difficult to industrialize such high-speed stirring; method 2, dissolving the crude ibrutinib in a mixed solvent of isopropanol and n-hepta...
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Abstract

The invention discloses a crystal form G of ibrutinib. The crystal form G is characterized in that X-ray powder diffraction (X-RPD) which adopts Cu-Kalpha radiation and is represented with a 2theta angle has diffraction peaks in positions at angles of 5.0 degrees plus or minus 0.2 degrees, 7.3 degrees plus or minus 0.2 degrees, 10.1 degrees plus or minus 0.2 degrees, 12.0 degrees plus or minus 0.2 degrees, 13.2 degrees plus or minus 0.2 degrees, 17.1 degrees plus or minus 0.2 degrees, 19.5 degrees plus or minus 0.2 degrees, 20.8 degrees plus or minus 0.2 degrees, 22.3 degrees plus or minus 0.2 degrees, 24.3 degrees plus or minus 0.2 degrees, 27.4 degrees plus or minus 0.2 degrees and 31.2 degrees plus or minus 0.2 degrees. Related solvents in a preparation process of the crystal form G are cheap, the conditions are mild, the operation is simple, good controllability and reproducibility are realized, further, the prepared crystal form has great stability, the HPLC (high performance liquid chromatography) purity is higher than 99%, and the phenomenon of crystal transformation can be avoided; besides, the solubility is high, the dissolubility is good, and the bioavailability is high.

Application Domain

Technology Topic

Crystal transformationSolvent +6

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  • Crystal form G of ibrutinib and preparation method
  • Crystal form G of ibrutinib and preparation method

Examples

  • Experimental program(1)
  • Effect test(1)

Example Embodiment

[0018] Example 1
[0019] Add 10g of Ibrutinib amorphous substance to 100ml of ethyl acetate and methanol mixed solution (the volume ratio of isopropanol and methanol is 2:1), heat to reflux to dissolve, after dissolution, stir for 10 hours, add 100ml of water, and stir for 2 After hours, filter, heat and dry while grinding to obtain crystal G, using Cu-Kα radiation, X-ray powder diffraction expressed in 2θ angles is as figure 1 As shown, the HPLC purity is 99.92%.
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