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Method for obtaining high-purity 17α-acetoxy-11β-(4-n,n-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione

A technology of dimethylaminophenyl and acetoxy, applied in the direction of steroids, organic chemistry, etc., can solve the problem of not being able to obtain high-purity Ulipristalacetate

Inactive Publication Date: 2011-12-28
SICHUAN UNIV
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  • Abstract
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Problems solved by technology

[0007] It has now been found that if the synthesis of Ulipristal acetate does not need to be purified in each step, it is directly used for the next step reaction, and the crude product of Ulipristal acetate is finally obtained as an oil, and then high-purity Ulipristal acetate cannot be obtained according to the purification operation of the aforementioned patent

Method used

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Examples

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Embodiment 1

[0016] Example 1 Obtaining relatively pure 17α-acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione solid

[0017] 20 g of 17α-acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione crude oil in a round bottom In the flask, at a temperature between 20°C and 100°C, add dioxane / n-hexane (the volume ratio of dioxane / n-hexane is between 0.01-50:1), stir, cool and precipitate a solid, and filter to obtain 15g off-white relatively pure 17α-acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione, HPLC The measured purity was 99%.

Embodiment 2

[0018] Example 2 Obtaining high-purity 17α-acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione solid

[0019] 15g of relatively pure 17α-acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione solid was used Methanol / water (methanol / water volume ratio is between 0.1 and 15) was stirred and dissolved at a temperature between 20°C and reflux, solids were precipitated after cooling, and filtered to obtain 13.5g of white 17α-acetoxy-11β-(4- N,N-Dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione. The purity measured by HPLC was 99.78%, and the single largest impurity was 0.05%.

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Abstract

The invention discloses a method of acquiring high-purity 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione, comprising the following steps: a) putting the acquired crude 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione in a proper solvent system to generate a pure 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione solid; b) separating the 17 alpha-acetoxy-11 beta-(4-N, N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione solid; and c) carrying out recrystallization on the acquired solid. The compound used as a new oral emergency contraception can be taken in 120 h after unprotected sexual intercourse of women without a reduction of emergency contraception effect with the delay of the time of using drugs, and has good safety and survivability simultaneously.

Description

technical field [0001] The present invention relates to obtaining high-purity 17α-Acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione, methods and uses thereof. Background technique [0002] Compound 17α-acetoxy-11β-(4-N,N-dimethylaminophenyl)-19-norpregna-4,9-diene-3,20-dione, common name: Ulipristal acetate, has the following formula: [0003] [0004] On August 13, 2010, the U.S. Food and Drug Administration (FDA) approved a new molecular entity emergency contraceptive tablet named Ella, and its drug name is Ulipristal acetate, which is an acetate salt. This emergency contraceptive tablet can be taken within 120 hours (5 days) after intercourse without measures. Ella is a progesterone receptor blocker / antagonist whose main function is to inhibit or delay female ovulation. In June 2010, the FDA's Advisory Committee for Reproductive Health Drugs discussed the drug. Members of the committee voted unanimously to approve Ela's marketing applicatio...

Claims

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Application Information

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IPC IPC(8): C07J7/00
Inventor 吴勇海俐余永国石浙秦李晓岑
Owner SICHUAN UNIV
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