Process for efficiently catalyzing synthesis of nicosulfuron nicotinamide intermediate

By combining a lanthanum-doped composite metal fluoride-diatomite supported catalyst with a 4A molecular sieve catalytic system, the problems of lengthy steps and high waste in the synthesis of dichloro-N,N-dimethylnicotinamide were solved, realizing a highly efficient and environmentally friendly catalytic synthesis of nicosulfuron-nicotinamide intermediates, which is suitable for industrial production.

CN122301767APending Publication Date: 2026-06-30JIANGSU FENGSHAN BIOCHEMICAL TECH CO LTD
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Patent Information

Application Number
CN202610610106.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-05-06
Publication Date
2026-06-30

AI Technical Summary

Technical Problem

The existing synthetic route for dichloro-N,N-dimethylnicotinamide is lengthy, generates a large amount of wastewater and waste, has high catalyst costs and insufficient stability, and has limited reaction equilibrium, making it difficult to achieve the target product with high conversion rate and high purity.

Method used

A lanthanum-doped composite metal fluoride-diatomite supported catalyst is used, combined with in-situ dehydration of 4A molecular sieve and pressurized excess dimethylamine gas, to achieve efficient catalysis in a liquid phase environment through amidation reaction. By utilizing the multi-metal active centers of the catalyst and the pore structure of the molecular sieve, combined with precise thermodynamic and kinetic control, the reaction is ensured to move towards the product, and high-purity products are obtained through post-processing refining.

Benefits of technology

A simple and efficient synthesis of dichloro-N,N-dimethylnicotinamide was achieved, reducing catalyst consumption and waste generation, improving reaction conversion rate and product purity, making it suitable for industrial production and meeting the requirements of green chemistry.

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Abstract

The invention discloses a process for efficiently catalyzing synthesis of a nicosulfuron nicotinamide intermediate in the technical field of organic synthesis. The process comprises the following steps: under the protection of nitrogen, adding a proper amount of dichloronicotinic acid, an organic solvent, a lanthanum-doped composite metal fluoride-diatomite supported catalyst and an encapsulated 4A molecular sieve into a reaction kettle; introducing nitrogen for replacement, and stirring after heating; introducing anhydrous dimethylamine gas, controlling the pressure, and continuously stirring for reaction; and after the reaction is finished, washing with a sodium bicarbonate aqueous solution, washing with deionized water, drying, concentrating and recrystallizing to obtain a target product. The lanthanum-doped composite metal fluoride-diatomite supported catalyst prepared by the invention can be recycled, has the advantages of mild reaction conditions and high product yield, is green and environment-friendly, and is suitable for industrial production.
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