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Method for preparing bilastine impurity

A technology of impurities and compounds, which is applied in the field of preparation of bilastine impurities, can solve problems such as the synthesis method of impurities that have not been reported in the literature, and achieve the effect of simple operation and high yield

Active Publication Date: 2017-01-25
NANJING CHANGAO PHARMA SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no literature report on the synthesis method of this impurity

Method used

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  • Method for preparing bilastine impurity
  • Method for preparing bilastine impurity
  • Method for preparing bilastine impurity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1 Compound II (R 3 for the preparation of ethyl)

[0017] At room temperature, 10 g of ethyl α,α-dimethyl-4-(2-bromoethyl)phenylacetate and 7 g of 2-(piperidin-4-yl)-1H-benzimidazole were dissolved in DMF (80 mL), Add 12g of diisopropylethylamine, raise the temperature to 60°C, stir for 5-6 hours, monitor the reaction by HPLC, cool to room temperature after the reaction, pour into the ice-water mixture, and stir for 30 minutes, suction filter, wash, The filter cake was dried under reduced pressure at 50° C. to obtain 8.4 g of off-white solid with a yield of 60%.

Embodiment 2

[0018] Example 2 Compound IV (R 3 is ethyl, R 1 For the preparation of methyl)

[0019] At 0°C, 8 g of compound II prepared in Example 1 was dissolved in DMF (50 mL), and 2.5 g of sodium hydrogen was added under nitrogen protection, stirred at room temperature for 1 hour, and compound III (R 1 is methyl, R 2 is bromine), after the dropwise addition, the temperature was raised to 60°C, and the stirring was continued for 4-5 hours. After the reaction was monitored by HPLC, it was cooled to room temperature, and the mixture of ice and water was slowly added, extracted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. Concentration gave 8 g of oily substance, yield 83%.

Embodiment 3

[0020] Example 3 Compound IV (R 3 is ethyl, R 1 For the preparation of methyl)

[0021] At 0°C, 8 g of compound II prepared in Example 1 was dissolved in THF (50 mL), and 8 g of sodium hydroxide was added under nitrogen protection, stirred at room temperature for 1 hour, and compound III (R 1 is methyl, R 2 is bromine), after the dropwise addition, the temperature was raised to 50°C, and stirring was continued for 5 hours. After the reaction was monitored by HPLC, it was cooled to room temperature, and a mixture of ice and water was slowly added, extracted with ethyl acetate, washed with water, dried over anhydrous sodium sulfate, and concentrated to obtain 8.3 g of oil, yield 86%.

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Abstract

The invention discloses a method for preparing a bilastine impurity A. The method comprises the following steps: (1) enabling a compound of a formula II as shown in the description to react with a compound of a formula III as shown in the description so as to generate a compound IV; (2) hydrating the compound IV to obtain a compound I, namely, the bilastine impurity A. By adopting the method, the bilastine impurity A can be obtained with a high yield, and can be used as an impurity reference substance in quality control of bilastine raw material medicines or preparations of the bilastine.

Description

technical field [0001] The invention belongs to the technical field of drug synthesis, and in particular relates to a preparation method of bilastine impurities. Background technique [0002] Bilastine is a second-generation oral non-sedative histamine H1 receptor antagonist, developed by Spanish FAES pharmaceutical company, approved by the European Union in 2010 for the treatment of allergic rhinitis and chronic idiopathic urticaria . The required dose of this product is small, the safety range is large, and it does not have the sedative effect on the central nervous system and the toxic and side effects on the cardiovascular system that commonly used antihistamines have. [0003] [0004] The lastine impurity A (shown in formula I) is produced by breaking the ether bond of bilastine under alkaline conditions. The impurity was detected in both commercially available and self-made tablets. Therefore, the synthesized high-purity bilastine impurity A can be used as an im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
CPCC07D401/04
Inventor 赵磊王晓林辉王正泽张丽林谢少斐李纬
Owner NANJING CHANGAO PHARMA SCI & TECH CO LTD
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