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A kind of preparation method of solifenacin succinate impurity

A technology of solifenacin succinate and impurities, which is applied in the field of preparation of solifenacin succinate impurity [formula (I)], can solve the problem that the compound preparation method is not reported in literature and the like, and achieves simple operation and simple reaction operation. , the effect of high product purity

Active Publication Date: 2017-11-17
天津市医药集团技术发展有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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By searching and investigating a large amount of related documents, the preparation method of the compound of the present invention has no bibliographical information

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  • A kind of preparation method of solifenacin succinate impurity
  • A kind of preparation method of solifenacin succinate impurity

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Embodiment 1

[0027] Get 5g of solifenacin succinate, stir and dissolve in the mixed solvent of 50ml of water and 5ml of acetone. Add 5.6g of potassium permanganate, stir at 20-25°C for 8h, and let stand overnight. The conversion rate of [2-(2-benzoyl-phenyl)-ethyl]-carbamic acid 1-aza-bicyclo[2.2.2]oct-3-yl ester was 45% by HPLC the next day. Filter, add 25ml of ethyl acetate for layering, adjust the pH to 9~10 with saturated potassium carbonate solution, and extract the aqueous layer with 25ml×2 ethyl acetate. The organic layers were combined and dried over anhydrous magnesium sulfate for 2 h. The desiccant was filtered off and concentrated under reduced pressure to obtain 3.4 g of a yellow oil. Separation by column chromatography (dichloromethane / methanol=15 / 1), TLC (dichloromethane / methanol=10 / 1) to monitor the separation process, collect the eluent, and concentrate under reduced pressure to dryness to obtain a white solid [2-(2 -Benzoyl-phenyl)-ethyl]-carbamic acid 1-aza-bicyclo[2.2...

Embodiment 2

[0030] Get 10g of solifenacin succinate, stir and dissolve in a mixed solvent of 100ml of water and 10ml of acetone. Add 11.2g of potassium permanganate, stir at 20-25°C for 8h, and leave overnight. The conversion rate of [2-(2-benzoyl-phenyl)-ethyl]-carbamic acid 1-aza-bicyclo[2.2.2]oct-3-yl ester was 54.6% by HPLC the next day. Filter, add 50ml of dichloromethane and 5% sodium hydroxide solution to adjust the pH to 9~10, separate the water layer, extract the water layer with 50ml×2 dichloromethane, combine the organic layers and dry with anhydrous magnesium sulfate for 2h. The desiccant was filtered off and concentrated under reduced pressure to obtain 6.5 g of a yellow oil. Separation by column chromatography (dichloromethane / methanol=15 / 1), TLC (dichloromethane / methanol=10 / 1) to monitor the separation process, collect the eluent, and concentrate under reduced pressure to dryness to obtain a white solid [2-(2 -Benzoyl-phenyl)-ethyl]-carbamic acid 1-aza-bicyclo[2.2.2]oct-3...

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Abstract

The present invention relates to a kind of solifenacin succinate impurity [2-(2-benzoyl-phenyl)-ethyl]-carbamic acid 1-aza-bicyclo[2.2.2]oct-3-yl ester method of preparation. It is obtained from solifenacin succinate through oxidative ring opening and separation and purification. The invention provides a reference substance for the qualitative and quantitative analysis of solifenacin succinate through the preparation of the impurity solifenacin succinate, effectively controls the quality of solifenacin succinate, and ensures the safety of clinical medication.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry and relates to a preparation method of solifenacin succinate impurity [formula (I)]. Background technique [0002] Solifenacin succinate [Formula (Ⅱ)], English name: Solifenacin succinate, trade name: Vesicare, is a new generation of highly selective M receptor developed by Japan Astellas Pharmaceutical Co., Ltd. (formerly Yamanouchi Pharmaceutical Co., Ltd.) Blocker is a drug used to treat symptoms of urinary incontinence and / or urinary frequency and urgency in patients with overactive bladder (OAB). The drug first went on the market in Europe in August 2004, and is currently on the market in more than 50 countries around the world. It was approved for marketing in China in 2009. [0003] [0004] The compound of the present invention [2-(2-benzoyl-phenyl)-ethyl]-carbamic acid 1-aza-bicyclo[2.2.2]oct-3-yl ester [formula (I)] is Japanese Ann A kind of ring-opening metabolite of so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D453/02
Inventor 杨汉跃郑家通陈学民陈琛孟庆礼李瑞敏
Owner 天津市医药集团技术发展有限公司
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