Polycrystalline type for ulipristal acetate and preparation method thereof
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A technology of ulipristal acetate and its polymorphism, which is applied in the field of polymorphism of ulipristal acetate, which can solve the problems of difficulty in obtaining high-purity products and helpless removal of impurities
Active Publication Date: 2014-04-30
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 1 g of ulipristal acetate crude product to 10-13 times the volume of ethanol (ml / g), heat to reflux to dissolve, add 0.1 g of activated carbon to decolorize, 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] Also switch to acetone, isopropanol, ethyl acetate, and crystallize to obtain different polymorphs of ulipristal acetate solvate.
preparation example 2
[0102] Preparation Example 2: Preparation method of ulipristal acetate isopropanol / ethanol solvate:
[0103] Add 1 g of crude ulipristal acetate to 10 times isopropanol / ethanol (9:1), heat to reflux to dissolve, add 0.1 g of activated carbon to decolorize, filter, then cool to 10°C while stirring, and stir for 30 minutes to 1 hour ,filter. Dry at 60°C to obtain 0.85 g of ulipristal acetate isopropanol / ethanol solvate, mp: 164-170°C.
[0105] Add 5 times of dichloromethane to dissolve 1 g of ulipristal acetate crude product, add 0.1 g of activated carbon to decolorize, filter, concentrate under reduced pressure to almost no solvent, add ethyl acetate / petroleum ether (1:5), and cool to 20°C After stirring for 30 minutes-1h, 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 a Chinese patent application with an application date of April 17, 2012, an application number of 201210112043.X, and an invention title of "polymorphic form of ulipristal acetate and its preparation method". technical field [0002] The present invention relates to polymorphic forms of ulipristal acetate, in particular to polymorphic forms A1 and polymorphic forms A2 of ulipristal acetate, an antiprogestogen and antiglucocorticoid drug, and a preparation method thereof. belongs to the field of medicinal chemistry. Background technique [0003] It is well known that different crystallization solvents or different crystallization methods will produce different polymorphic forms, and different polymorphic forms have different stability and solubility, and sometimes even have different bioavailability in vivo. Therefore, it is very necessary to find a highly pure and stable polymorph in drug development, and the method is e...
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