Polymorphic form of ulipristal acetate and preparation method thereof
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A technology of ulipristal acetate and polymorphic forms, applied in the field of polymorphic forms of ulipristal acetate, can solve problems such as difficulty in obtaining high-purity products, helpless removal of impurities and the like
Active Publication Date: 2018-01-02
CHANGZHOU NO 4 PHARMA FACTORY +1
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[0013] The above-mentioned method of crystallization with ethanol / water to obtain a solvate-free product actually does not help crystallization to remove impurities, and even new impurities are produced due to long-term high-temperature heating, so it is more difficult to obtain high purity with a single impurity below 0.1%. product
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preparation example 1
[0099] Preparation Example 1: General preparation method of ulipristal acetate solvate polymorph:
[0100] Add 1g of crude ulipristal acetate to 10-13 times ethanol (ml / g), heat to reflux to dissolve, add 0.1g activated carbon for decolorization, filter, concentrate under reduced pressure to 3-5 times the volume, and then cool to After stirring at 10°C for 30 minutes to 1 hour, filter. Dry at 60°C. Obtained 0.88 g of ulipristal acetate ethanolate, mp: 150-170°C.
[0101] Similarly, acetone, isopropanol, and ethyl acetate were used for crystallization to obtain different polymorphs of ulipristal acetate solvate.
[0103] Add 1g of crude ulipristal acetate into 10 times isopropanol / ethanol (9:1), heat to reflux to dissolve, add 0.1g activated carbon for decolorization, filter, then cool to 10℃ under stirring, and stir for 30 minutes-1h. ,filter. Dry at 60°C to obtain 0.85 g of ulipristal acetate isopropanol / ethanol solvate, mp: 164-170°C.
preparation example 3
[0104] Preparation Example 3: Preparation method of ulipristal acetate ethyl acetate / petroleum ether solvate:
[0105] Dissolve 1g crude ulipristal acetate with 5 times dichloromethane, add 0.1g activated carbon to decolorize, filter, concentrate under reduced pressure to almost no solvent, add ethyl acetate / petroleum ether (1:5), cool to 20°C After stirring for 30 minutes to 1 hour, filter. Dry at 60°C to obtain 0.85 g of ulipristal acetate ethyl acetate / petroleum ether solvate, mp: 160-210°C.
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Abstract
The invention discloses a polycrystalline type A1 and a polycrystalline type A2 of ulipristal acetate (shown as a formula I) not containing any solvate, and preparation methods, a medicinal composition and medicinal application thereof. As proved by smelting point, X-ray powder diffraction (XRD), infrared spectrogram (IR), differential thermal analysis spectrogram (DSC) and thermal weight loss spectrogram (TG), the polycrystalline type A1 and the polycrystalline type A2 of ulipristal acetate prepared by using the methods are extremely stable under the conditions of temperature, illumination and moisture, and contribute to long-time storage. A used crystallization solvent is safe and is easy to remove, the prepared polycrystalline type A1 and polycrystalline type A2 can be directly applied to preparation processing, and the preparation methods are easy to operate, and suitable for industrial production.
Description
[0001] This application is a divisional application of the Chinese patent application with the application date of April 17, 2012, the application number 201210112043.X, and the name of the invention "polymorph of ulipristal acetate and its preparation method". Technical field [0002] The invention relates to a polymorphic form of ulipristal acetate, in particular to a polymorphic form A1 and polymorphic form A2 of an anti-progestin and anti-glucocorticoid drug ulipristal acetate and a preparation method thereof. It belongs to the field of medicinal chemistry. Background technique [0003] As we all know, different crystallization solvents or different crystallization methods will produce different polymorphs, and different polymorphs have different stability and solubility, and sometimes even have different bioavailability in the body. Therefore, it is necessary to find a high-purity and stable polymorph in drug development, and the method is easy to reproduce and is suitable fo...
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