Polycrystal forms 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: 2012-09-19
CHANGZHOU NO 4 PHARMA FACTORY +1
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[0012] The above-mentioned method of crystallization with ethanol/water to obtain a solvate-free product actually does not help crystallization to remove impurities, and
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preparation example 1
[0098] Preparation Example 1: General preparation method of ulipristal acetate solvate polymorph:
[0099] 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.
[0100] Also switch to acetone, isopropanol, ethyl acetate, and crystallize to obtain different polymorphs of ulipristal acetate solvate.
preparation example 2
[0101] Preparation Example 2: Preparation method of ulipristal acetate isopropanol / ethanol solvate:
[0102] 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.
[0104] 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 polycrystal form A1 and a polycrystal form A2 of ulipristal acetate (formula I) free of solvate and a preparation method, a pharmaceutical composition and medical application of the polycrystal forms. By verification of melting point, X-ray diffraction powder spectrum (XRD), infrared spectrum (IR), differential thermal analysis spectrum (DSC) and thermogravimetric spectrum (TG), the polycrystal form A1 and polycrystal form A2 of ulipristal acetate prepared by the method disclosed by the invention are extremely stable to temperature, illumination and humidity, and favorable to long-term storage; the used crystallizing solvent is safe and easy to remove; the obtained polycrystal form A1 and the polycrystal form A2 can be directly used for preparation processing; and the preparation method is simple in operation and suitable for industrial production. The formula I is shown in the description.
Description
technical field [0001] 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 [0002] 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 easy to reproduce and suitable for industrial large-scale preparation. In addition, X-diffraction powder pattern (XRD) is an effective means to determine the crystal form. [0003] Ulipristal acetate; compound I; chemical name: 17α-acetoxy-11β-(4-N,N-dimethylaminop...
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