Preparation method of mizolastine intermediate

By using specific molar ratio reactions of BBMZ, PD and organic base in the preparation process of imidazostin intermediates, and combining organic solvent dissolution, filtration, crystallization and crystal cultivation steps, problems such as long reaction time and low yield in traditional processes are solved, and an efficient and environmentally friendly preparation method is achieved, and the purity and yield of the product are improved.

CN119707917AActive Publication Date: 2025-03-28SHENYANG SANJIU PHARMA +1
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Patent Information

Application Number
CN202411907339.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-24
Publication Date
2025-03-28
Estimated Expiration
2044-12-24

AI Technical Summary

Technical Problem

The preparation process of traditional imidazostin intermediates has problems such as long reaction time, low yield, cumbersome operating procedures, many impurities, high environmental pressure, and easy product adhesion.

Method used

BBMZ, PD and organic alkali are mixed in a specific molar ratio, and the reaction temperature is controlled at 80~100°C, and the reaction time is 3-5 hours. The addition of organic solvents is then used to promote dissolution, and the by-products are removed by filtration, and high-quality PDA products are obtained through crystallization and crystal cultivation steps, and the process is simplified by air drying.

Benefits of technology

It has achieved a shortening of reaction time and high reaction conversion rate, simplified the operation process, reduced resource waste and environmental pollution, improved the purity and yield of the product, and solved the product adhesion problem.

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Abstract

The invention discloses a preparation method of an mizolastine intermediate, relates to the technical field of medicines, and aims to solve the problems of complex synthesis process and low conversion rate of the mizolastine intermediate. The preparation method comprises the following steps: S1, reaction: mixing BBMZ, PD and organic alkali according to the molar ratio of 1: (1.0-2.0): (0.8-1.2), and reacting at the temperature of 80-100 DEG C for 3-5 hours; s2, dissolving: adding an organic solvent which is 1-3 times of the weight of the reaction mixture into the reaction mixture to promote the dissolution of a reaction product; s3, filtering: filtering to remove hydrochloride of the by-product organic alkali; s4, crystallization: adding 0.5-2 times by weight of water into the filtrate, stirring and crystallizing, and controlling the temperature range to be 20-45 DEG C; s5, growing crystal: cooling the solution to 0-10 DEG C, and continuously stirring for not less than 1 hour; s6, filtering and washing: washing a filter cake by using an organic solvent and water in sequence; and S7, drying: performing forced air drying on the washed filter cake at the temperature of 20-30 DEG C for 5-6 hours to obtain a PDA product. According to the method, the production efficiency and the product quality are improved, the environmental influence is remarkably reduced, and the method has important industrial application value.
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