Ibrutinib amorphous substance and medicinal composition thereof
A technology of ibrutinib and amorphous substances, which is applied in the amorphous field of pharmaceutical compounds, can solve the problems of affecting the bioavailability, solubility and stability of drugs, affecting the dissolution and release of pharmaceutical compositions, etc.
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Embodiment 1
[0061] Take 10g 1-[3(R)-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl]piperidin-1-yl ]-2-propen-1-one was dissolved in 60ml of tetrahydrofuran, and the above solution was added to 120ml of isopropanol, and the above mixed solution was added to 600ml of n-heptane cooled to -20°C, and a white viscous substance was precipitated under stirring, poured The liquid is discharged, dried under reduced pressure, and the amorphous substance of ibrutinib can be collected, and the X-ray diffraction pattern of the product obtained is as follows: figure 1 shown.
Embodiment 2
[0063] Take 30g 1-[3(R)-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl]piperidin-1-yl ]-2-propen-1-one was dissolved in 300ml of dichloromethane, stirred and dissolved at room temperature; concentrated and dried under reduced pressure to obtain the amorphous substance of ibrutinib, and the X-ray diffraction spectrum of the product obtained was the same as in Example 1 Basically the same.
Embodiment 3
[0064] The prescription and preparation technology of embodiment 3 capsules:
[0065] The above 1-[3(R)-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidine- 1-yl]piperidin-1-yl]-2-propen-1-one amorphous was formulated into capsules containing 140 mg per tablet, and the results are shown in Table 6.
[0066] Table 6 Prescription situation
[0067]
[0068] Preparation process: containing 1-[3(R)-[4-amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl]piperidine-1 -base]-2-propen-1-one amorphous capsules are manufactured by combining the above-mentioned excipients with 1-[3(R)-[4-amino-3-(4-phenoxyphenyl)- The amorphous 1H-pyrazolo[3,4-d]pyrimidin-1-yl]piperidin-1-yl]-2-propen-1-one is mixed uniformly by the method of increasing the equal amount, and filled into capsules. The reference crystals were mixed and filled into capsules in the same manner. Table 7 shows the comparison of dissolution test results of capsule formulations
[0069] Table 7 Comparison of...
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