Ulipristal acetate crystals and preparation method thereof

A technology of ulipristal acetate and crystals, which is applied in the field of pharmaceuticals, can solve problems such as unsatisfactory crystal purity, and achieve the effects of good solubility, simple operation, and strong thermal stability

Active Publication Date: 2013-01-23
SHANDONG CHENGCHUANG BLUE OCEAN PHARM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purity of the crystal forms prepared in the above inventions is not ideal

Method used

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  • Ulipristal acetate crystals and preparation method thereof
  • Ulipristal acetate crystals and preparation method thereof
  • Ulipristal acetate crystals and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 25 g of crude ulipristal acetate and 50 ml of ethyl acetate to the reaction flask, heat to reflux for 30 minutes, perform hot filtration at 60°C, cool to -20°C to crystallize, and filter to obtain a white solid. Take the above white solid, add 50ml of water, stir, heat to 30°C, stir for 30 minutes, filter while hot, and dry under vacuum to obtain 20.2g of ulipristal acetate with a yield of 80.8% and a purity of HLPC of 99.75%.

Embodiment 2

[0036] Add 25 g of crude ulipristal acetate and 1250 ml of ethyl acetate to the reaction flask, heat to reflux for 10 hours, heat filter at 70°C, cool down to 0°C to crystallize, filter to obtain a white solid. Take the above white solid, add 1250ml of water, stir, heat to 50°C, stir for 30 minutes, filter while hot, and dry under vacuum to obtain 22.3g of ulipristal acetate with a yield of 89.2% and a purity of HLPC of 99.80%.

Embodiment 3

[0038] Add 25 g of crude ulipristal acetate and 500 ml of ethyl acetate to the reaction flask, heat to reflux for 5 hours, heat filter at 60°C, cool to -10°C to crystallize, filter to obtain a white solid. Take the above white solid, add 650ml of water, stir, heat to 40°C, stir for 30 minutes, filter while hot, and dry under vacuum to obtain 21.9g of ulipristal acetate with a yield of 87.6% and a purity of HLPC of 99.83%.

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PUM

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Abstract

The invention provides ulipristal acetate crystals. In the powder X ray of diffraction pattern of the crystals radiated by copper Ka rays with wavelength lambda being 1.54 angstroms, obvious main peaks appear at distances from the surface of the crystal surface (d) equals to 19.70+ / -0.05, 14.72+ / -0.05, 9.86+ / -0.05, 7.77+ / -0.05, 7.16+ / -0.05, 6.45+ / -0.05, 5.96+ / -0.05, 5.43+ / -0.05, 5.21+ / -0.05, 4.86+ / -0.05, and 4.31+ / -0.05. Compared with the conventional crystals, the ulipristal acetate crystals are more pure and stable. The invention also provides a method for preparing the crystals. The method comprises the following steps of: recrystallizing ulipristal acetate in a soluble solvent; washing the crystals in a solvent; and drying the crystals in vacuum to obtain finished products. The preparation method is characterized by simple operation and high product purity.

Description

technical field [0001] The present invention relates to a medicine, in particular to a novel crystal of the medicine, more specifically to a novel crystal of ulipristal acetate, a novel birth control drug. The present invention also relates to the preparation method of the novel crystal of the drug. Background technique [0002] Ulipristal acetate Chemical name: 17α-Acetoxy-11β-[4-N,N-Dimethylaminophenyl]-19-norpregna-4,9-diene-3,20-dione , the structural formula is: [0003] [0004] Ulipristal acetate was originally developed by RES TRIANGLE INST in the United States, and later authorized by HRA Pharma in France. The product of HRA Pharma was launched in Europe on March 2009. The English name is ulipristal acetate, also known as CDB-2914 , is a selective progesterone receptor modulator. The European Medicines Agency has approved this variety for emergency contraception within 120 hours of unprotected intercourse or contraceptive failure. It was listed in the Unite...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J41/00
Inventor 李建兵冯艾平张兴亮
Owner SHANDONG CHENGCHUANG BLUE OCEAN PHARM TECH CO LTD
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