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A kind of purification method of high-purity bepotastine besylate

A technology of bepotastine benzenesulfonate and a refining method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as inability to effectively remove impurity A, inability to effectively remove impurities, and inability to recover and repurify. , to achieve the effect of low production cost, cost saving and simple operation

Active Publication Date: 2019-08-02
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Experiments have proved that this method can effectively remove impurities B, C, D, E, F, but not impurities A, G
[0014] Existing refining methods cannot effectively remove impurity A, and refining with alcohol solvents will introduce benzenesulfonate genotoxic impurities
The crude product recovered from the crystallization mother liquor cannot be recycled and refined, which is a serious waste and high cost

Method used

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  • A kind of purification method of high-purity bepotastine besylate
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  • A kind of purification method of high-purity bepotastine besylate

Examples

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Effect test

Embodiment 1

[0062] The refining method of high-purity bepotastine bepotastine in the present embodiment comprises the following steps:

[0063] 1. Add 20 g of crude bepotastine besilate to 200 ml of acetonitrile, heat to 80°C, stir to dissolve and filter, cool the filtrate to 25-30°C, stir and crystallize for 6 hours, filter, and dry the filter cake at 60°C under reduced pressure After 4 hours, 18.3 g of the primary refined product was obtained, with a yield of 91.5% and a purity of 99.89%.

[0064] 2. Add 18g of the primary refined product to 90ml of water, heat to 30-40°C, stir to dissolve, cool to -1-5°C, stir and crystallize for 6h, filter, and dry the filter cake at 40°C for 12h under reduced pressure to obtain benzenesulfonate Bepotastine pure product 16.3g, yield 90.6%, purity 99.99%.

Embodiment 2

[0066] 1. Add 20 g of crude bepotastine besilate to 300 ml of acetonitrile, heat to 60°C, stir to dissolve and filter, cool the filtrate to 10-20°C, stir and crystallize for 8 hours, filter, and dry the filter cake at 50°C under reduced pressure After 5 hours, 18.4 g of the primary refined product was obtained, with a yield of 92% and a purity of 99.90%.

[0067] 2. Add 18g of the primary refined product to 35ml of water, heat to 70°C, stir to dissolve, cool down to -1-5°C, stir and crystallize for 4h, filter, and dry the filter cake at 50°C for 10h under reduced pressure to obtain bezulbeta The pure product of Sting is 16.4g, the yield is 91.1%, and the purity is 99.96%.

Embodiment 3

[0069] 1. Add 100g of crude bepotastine besilate to 1000ml of acetonitrile, heat to 90°C, stir to dissolve and filter, cool the filtrate to 20-30°C, stir and crystallize for 6h, filter, and dry the filter cake at 70°C under reduced pressure After 4 hours, 92.8 g of the primary refined product was obtained, with a yield of 92.8% and a purity of 99.88%.

[0070] 2. Add 92g of the primary refined product to 270ml of water, heat to 50°C, stir to dissolve, cool down to -1-5°C, stir and crystallize for 5h, filter, and dry the filter cake at 55°C for 10h under reduced pressure to obtain besylate The pure product of Sting is 84.8g, the yield is 92.2%, and the purity is 99.97%.

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Abstract

The invention discloses a refining method for high-purity bepotastine besilate. The refining method is a solvent crystallization method adopting a crude bepotastine besilate product as a raw material and comprises the following steps: firstly, the crude bepotastine besilate product is heated and dissolved with acetonitrile and filtered, a filtrate is cooled, stirred and crystallized, crystals are filtered and dried, and primary refined product is obtained; the primary refined product is heated, stirred, dissolved in water and filtered, a filtrate is cooled, stirred and crystallized, crystals are filtered and dried, and a pure bepotastine besilate product is obtained. The method has the advantages that the operation is simple and convenient, the yield is high, the product is pure, the cost is saved and the like, the total yield is 80% or higher, the purity of the pure bepotastine besilate product is 99.9% or higher proved by HPLC detection, the isomer impurity content is reduced to 0.1% or lower from 0.4%, and other single impurity content is reduced to 0.1% or lower from 0.2%.

Description

[0001] 1. Technical field [0002] The invention relates to a method for purifying chemical drugs, in particular to a method for refining high-purity bepotastine besilate. [0003] 2. Technical background [0004] Bepotastine Besilate, the chemical name is (+)-(S)-4-{4-[(4-chlorophenyl)(2-pyridine)methoxy]piperidine}butyric acid benzene Sulfonate, chemical structural formula sees following formula I: [0005] [0006] Bepotastine besilate is a histamine H 1 Receptor antagonist, jointly developed by Japan Tanabe Seiyaku Pharmaceutical Co., Ltd. and Japan Ube Industries Co., Ltd. Bepotastine besilate tablets (trade name: 5mg, 10mg) were first listed in Japan in 2000, and are mainly used clinically for the treatment of itching caused by allergic rhinitis, urticaria and skin diseases (eczema, dermatitis, prurigo, pruritus). [0007] There is a chiral center in the molecule of bepotastine besilate, namely (4S)-(4-chlorophenyl)(2-pyridine)methoxypiperidine structure. And the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D401/12C07C309/73C07C303/44
CPCC07C303/44C07D401/12C07C309/73
Inventor 吴标凌林戴一张严金
Owner HEFEI JIUNUO MEDICAL TECH
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