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Preparation method of bepotastine besilate

A technology of bepotastine benzenesulfonate and hydrochloric acid is applied in the preparation of sulfonates, chemical instruments and methods, feeding devices, etc., and can solve problems such as difficulty in the method of purity

Inactive Publication Date: 2019-10-25
浙江天顺药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are very few reports about improving the purity of bepotastine besylate in the existing relevant literature, and recrystallization is often used for purification
Although the recrystallization method can obtain bepotastine bepotastine with a purity of 95%, further purification is required to obtain bepotastine with a purity of more than 99%, and the optical isomers are controlled below the detection limit. The method of purity is very difficult

Method used

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  • Preparation method of bepotastine besilate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1, 100 g of the crude bepotastine besylate was added to 400 ml of an aqueous solution containing 40 g of potassium carbonate, cooled to 5-10° C., stirred until the solution was clear, and filtered to obtain a clear solution;

[0025] Add 100ml of dichloromethane to the solution, extract, separate, remove the water phase, then add 100ml of toluene, extract, separate, and collect the organic phase;

[0026] Add 96ml of 5mol / L hydrochloric acid to the organic phase, and slowly precipitate solids as the acid is added. During the dropping process, the temperature is controlled at 5-10°C, the pH is controlled at 8, and the stirring time is 30min;

[0027] Add the filtered solid to 1000mL water to make a slurry for 2h, filter, and repeat once;

[0028] The final obtained solid was added to a vacuum drying oven, and dried under reduced pressure at 85° C. for 24 hours (desiccant P2O5) to obtain 69 g of the product, with a yield of 69%. The purity of the final product is...

Embodiment 2

[0029] Example 2, add 100 g of crude bepotastine besilate to 400 ml of an aqueous solution containing 100 g of sodium carbonate, cool down to 5-10° C., stir until the solution is clear, and filter to obtain a clear solution.

[0030] Add 400ml of dichloromethane into the solution, extract, separate the liquid, remove the water phase, add 400ml of toluene therein, extract, extract, separate the liquid, and collect the organic phase;

[0031] Add 96ml of 5mol / L hydrochloric acid to the organic phase, and slowly precipitate solids with the addition of acid. During the dropping process, the temperature is controlled at 5-10°C, the pH is controlled at 7, and the stirring time is 30min;

[0032] The resulting solid was added to 5000mL water to make a slurry for 2h, filtered, and then repeated once;

[0033] The final obtained solid was added to a vacuum drying oven, and dried under reduced pressure at 85° C. for 24 hours (desiccant P2O5) to obtain 66 g of the product, with a yield o...

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Abstract

The invention discloses a preparation method of bepotastine besilate, and belongs to the fields of organic chemistry and medicinal chemistry. The preparation method comprises the following steps: performing alkali dissolution by using crude bepotastine besilate as a raw material, performing organic solvent extraction, performing acid crystallization, performing beating, performing filtration, andperforming drying to obtain the high-purity bepotastine besilate. The method provided by the invention effectively solves the technical problems of a high content of impurities and low purity of the crude bepotastine besilate, and has the advantages of a simple process and low costs.

Description

technical field [0001] The invention belongs to the fields of organic chemistry and medicinal chemistry, and in particular relates to a preparation method of bepotastine besylate. Background technique [0002] Bepotastine, chemical name (+)-4-[[(S)-p-chloro-α-2-pyridylbenzyl]oxy]-1-piperidine butanoic acid, English name Bepotastine, clinical Bepotastine Bepotastine is marketed with bepotastine besylate as the active ingredient. Bepotastine besylate is the besylate salt of bepotastine, a drug with antihistamine activity that can be used to treat Allergic diseases such as rhinitis, and skin diseases such as eczema, dermatitis, prurigo, itchy skin, and urticaria. [0003] Existing studies have shown that different isomers of bepotastine besylate have significant differences in pharmacological effects, among which the S isomer has more than 100 times stronger pharmacological effects than the R isomer, and the S isomer binds to plasma proteins The rate is higher than that of th...

Claims

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Application Information

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IPC IPC(8): C07D401/12C07C303/32C07C309/29B01J19/18B01J4/00
CPCB01J4/001B01J19/0053B01J19/18C07C303/32C07D401/12C07C309/29
Inventor 张胜
Owner 浙江天顺药业有限公司
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