Entrectinib crystal form and preparation method thereof
A technology of entrectinib and crystal forms, applied in the field of medicinal chemistry, can solve the problems of poor stability of crystal forms, poor solubility of crystal forms 2 and 4, etc.
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[0226] (3) The preparation process of the crystal form AZT-A is simple, the operability is strong, the yield is high, the quality is stable, the production cycle is short, and it is easy to realize large-scale production.
[0227] (4) Compared with the amorphous form, the crystal form AZT-A is less likely to raise dust, has better stability under high humidity and / or high temperature, is less hygroscopic and has good fluidity, and is suitable for formulation technology.
[0228] Crystal form AZT-B of entrectinib and preparation method thereof
[0229] In a specific embodiment, the crystal form of entrectinib provided by the present invention is crystal form AZT-B.
[0230] In another preferred embodiment, the crystalline form AZT-B is the anhydrate of entrectinib.
[0231] In a specific embodiment, under powder X-ray diffraction, the crystalline form AZT-B has characteristic peaks at 2θ of 7.4±0.2°, 8.1±0.2°, 14.8±0.2°, 17.2±0.2°, 19.9±0.2° .
[0232] In another preferred e...
Embodiment 1
[0467] Preparation of Entratinib Crystal Form AZT-A
Embodiment 1-1
[0469] Mix 2 g of Entratinib crystal form 2 with 10 ml of ethyl acetate, heat to 50°C to dissolve, cool to 10°C, and dry at room temperature to obtain crystal form AZT-A. Its X-ray powder diffraction pattern is as follows figure 1 shown; the obtained solid is tested by TGA and its spectrum is as follows figure 2 As shown; the obtained solid is subjected to DSC test and its spectrum is as follows image 3 shown; the obtained solid was subjected to 1 H-NMR test, its spectrum is as follows Figure 4 shown.
[0470] figure 2 TGA showed that the crystalline form AZT-A lost 0.3% in weight at 30°C-150°C and was anhydrous.
[0471] image 3 DSC showed that the crystalline form AZT-A had the first endothermic peak at 162.5 °C and the second endothermic peak at 196.78 °C.
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Abstract
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