High-purity ulipristal acetate

A high-purity technology of ulipristal acetate, applied in the field of high-purity ulipristal acetate compounds, can solve problems such as failure to prepare a single crystal form A crystal product of ulipristal acetate, and achieve high crystal yield , Simple operation, stable process effect

Inactive Publication Date: 2015-03-18
SICHUAN HAISCO PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0036] Therefore, in the existing disclosed technology, in fact, it has not been possible to prepare a completely pure single crystal form A ulipristal acetate crystal product

Method used

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Examples

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Effect test

preparation example Construction

[0065] Preparation of single crystal A:

[0066] Ulipristal acetate is dissolved in methanol aqueous solution, and the solid is slowly volatilized at rest, and the large particle solid is taken as single crystal A. In this operation mode, single crystals of milligram level can be obtained each time.

[0067] Preparation of crystal type A seed crystals:

[0068] Ulipristal acetate was added to 50-80% methanol aqueous solution, heated to reflux to dissolve, cooled by adding single crystal A to induce, slowly cooling down to gradually precipitate crystals, and the obtained crystals were used as crystal type A seed crystals. In this operation mode, gram-level seeds can be obtained every time.

Embodiment 1A

[0069] Example 1A Preparation of Crystal Form Ulipristal Acetate

[0070] Take 8L prepared 30% (V Ethanol :V water =30:70) Ethanol aqueous solution, add 200g crude ulipristal acetate under stirring, heat up to reflux to dissolve, after dissolving, filter to remove mechanical impurities, the filtrate will continue to heat up to fully dissolved, cool to 50℃, add seed crystals under stirring 8g. Slowly cool down and gradually precipitate crystals, continue to cool to 0~5℃, filter, and dry under vacuum at 40~50℃ to obtain 160g of ulipristal acetate. The content of ulipristal acetate measured by HPLC is 99.85%, the largest single impurity The content is 0.05%. After X-ray powder diffraction test (using Cu-K radiation), the X-ray powder diffraction spectrum is as follows Picture 9 As shown, the diffraction data is shown in Table 4 below.

[0071] Table 4 X-ray powder diffraction data of crystalline form A ulipristal acetate prepared in Example 1

[0072]

Embodiment 2A

[0073] Example 2A Preparation of Crystal Form Ulipristal Acetate

[0074] Take 10L prepared 60% (V Ethanol :V Methanol :V water =40:20:40) Alcohol aqueous solution, add 400g crude ulipristal acetate under stirring, heat up to reflux to dissolve, filter to remove mechanical impurities after dissolving, continue to heat up the filtrate to fully dissolved, cool to 60°C, add under stirring Seed crystal 10g. Slowly lower the temperature and gradually precipitate crystals, continue to lower the temperature to 0~5℃, filter, and dry under vacuum at 40~50℃ to obtain 310g of ulipristal acetate. The X-ray powder diffraction test shows that Picture 9 Shown are consistent X-ray powder diffraction patterns.

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Abstract

The invention discloses a high-purity ulipristal acetate compound and a preparation method thereof. The preparation method comprises steps of dissolving, cooling, adding a crystal seed, continuing to cool, filtering the crystal, baking to dry and the like. The prepared ulipristal acetate crystal is a high-purity single A-crystal-form product with excellent stability. The preparation method has the advantages of high crystal yield, simple operation, stable technology and the like, and is suitable for industrialized production.

Description

Technical field [0001] The invention belongs to the field of medicinal chemistry, and specifically relates to a high-purity ulipristal acetate compound. Background technique [0002] Ulipristal acetate, chemical name: 17α-acetoxy-11β-[4-(N,N-dimethyl-amino)-phenyl]-19-norgestrel-4, 9-diene-3,20-dione, whose structure is shown in formula I, can be prepared according to the method disclosed in WO8912448. [0003] [0004] Ulipristal acetate is a steroid with anti-pregnancy and anti-glucocorticoid activity. It is a selective progesterone receptor modulator and is suitable for contraceptive gynecological indications, Cushing's syndrome and glaucoma. Ulipristal acetate was developed by Labora-toire HRA Pharma in France, and was approved by the US FDA in August 2010. The trade name is Ella. It is the world's first drug approved for emergency contraception within 120 hours; February 2012, The European Commission approved the Ulipristal Acetate 5 mg tablet Esmya developed by Gedeon Richt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J41/00
CPCC07J41/005
Inventor 童雷许战锋万华牛斌程睿
Owner SICHUAN HAISCO PHARMA CO LTD
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