A method for continuous synthesis of 2-methyl-5-nitroimidazole by nitration

By combining a microchannel reactor and a delayed-time reactor and adopting low-temperature nitration technology, the safety and environmental protection issues of high-temperature nitration in the existing technology are solved, and the industrial production of high-purity and high-yield 2-methyl-5-nitroimidazole is achieved.

CN119775210BActive Publication Date: 2025-09-19TAIZHOU PUDU MASCH EQUIP CO LTD
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Patent Information

Application Number
CN202510274576.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-03-10
Publication Date
2025-09-19
Estimated Expiration
2045-03-10

AI Technical Summary

Technical Problem

The existing technology has problems such as high reaction temperature, high energy consumption, high risk and poor environmental protection in the process of synthesizing 2-methyl-5-nitroimidazole, and the existing method is not suitable for industrial production.

Method used

A microchannel reactor is used for nitration reaction, and a jet fish structure microchannel reactor is used for low-temperature nitration. Combined with the control of concentrated sulfuric acid and fuming nitric acid, the reaction temperature is controlled below 50°C through the combination of a microchannel reactor and a delayed reactor, and crystallization treatment is carried out by adjusting the pH value.

Benefits of technology

A safe and stable low-temperature nitration reaction is achieved, which reduces the requirements for equipment materials, reduces the amount of fuming nitric acid used, avoids brown-yellow smoke, improves the mixing effect and heat exchange efficiency, ensures the continuity and safety of the reaction, and achieves product purity and yield of over 99.8%.

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Abstract

The invention discloses a method for continuously synthesizing 2-methyl-5-nitroimidazoles by nitration, comprising the steps of: S1, dissolving 2-methylimidazole in concentrated sulfuric acid, adding acetic anhydride, configuring solution A for standby, 2-methylimidazole must first be dissolved in concentrated sulfuric acid and the temperature does not exceed 40 DEG C; S2, adding ammonium sulfate to concentrated sulfuric acid and fuming nitric acid, configuring solution B for standby, the temperature of ammonium sulfate dissolved in fuming nitric acid does not exceed 30 DEG C; S3, solution A is pumped into a microchannel reactor, and solution B is pumped into a microchannel reactor; nitration reaction is carried out; S4, the reaction solution output from the microchannel reactor is added to water, the pH value is adjusted, and the temperature is reduced and crystallized, filtered, washed, and dried to obtain 2-methyl-5-nitroimidazoles. The method of the present invention is used to reduce the requirements of high-temperature nitration reaction on equipment materials, reduce the amount of fuming nitric acid used, and the reaction process is safe and stable. The 2-methyl-5-nitroimidazoles prepared by the method have higher purity.
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