Production process of sulfachloropyridazine

Abstract

The invention discloses a production process of sulfachloropyridazine. The production process comprises the following steps: S1, stirring and mixing 3, 6-dichloropyridazine, sulfanilamide, potassium carbonate and tri-n-propylamine, heating to 140-150 DEG C, and keeping the temperature for 4-5 hours; S2, carrying out high performance liquid chromatography detection, and terminating the condensation reaction if the mass content of sulfanilamide in the material is less than 10%; S3, adding water and activated carbon, controlling the temperature to 90-95 DEG C, keeping the temperature for 2 hours, decolorizing, then taking out the material, filtering, collecting filtrate, adjusting the pH value of the filtrate to 5-6 at 20-30 DEG C so as to separate out crystals, and centrifugally drying to obtain a crude product; S4, adding water into the crude product, adjusting the pH value of the crude product to 13-14, adding activated carbon, heating to 90-95 DEG C, keeping the temperature for 2 hours, decolorizing, taking out the material, filtering, collecting filtrate, adjusting the pH value of the filtrate to 5-6 at a temperature of 20-30 DEG C so as to separate out crystals, and centrifugally drying to obtain fine sulfachlorpyridazine; and S5, cooling the crude product mother liquor to 0-5 DEG C to separate out sulfanilamide, wherein the refined mother liquor is recycled and mixed with the water and the activated carbon in the step S3.

Description

technical field [0001] The invention relates to the field of pharmaceutical technology, in particular to a production process of sulfachloropyridazine. Background technique [0002] Sulfa drugs are the earliest synthetic antibacterial drugs, usually white or light yellow crystalline powder. Since the invention and application in the 1930s, sulfa drugs have been widely valued and studied as the most valuable antibacterial drugs due to their advantages of easy production, easy storage, good efficacy, convenient use, and low price. . Sulfonamide drugs have a history of more than 80 years, and more than 8,500 kinds of sulfonamide drugs have been synthesized successively. More than 20 kinds of sulfamethoxine, sulfamethoxine, and sulfamethazine are commonly used in clinical practice. With the continuous discovery and development of various antibiotics, antibiotics and quinolones have gradually replaced sulfa drugs, but sulfa drugs still have their unique advantages, such as wide...

AI Technical Summary

Problems solved by technology

However, there are certain difficulties in the follow-up treatment after adding high-boiling solvents, and some catalysts will make the reactants darker, which is not conducive to the production activities of enterprises.