Production process of sulfachloropyridazine

A sulfachloropyridazine and production process technology, applied in the field of sulfachloropyridazine production process, can solve problems such as unfavorable production activities of enterprises, darkening of reactant color, difficult treatment, etc., and achieve reduction of sewage generation, mild reaction, and equipment simple effect

Pending Publication Date: 2021-11-19
佛山市南海北沙制药有限公司
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Problems solved by technology

However, there are certain difficulties in the follow-up treatment after adding high-boiling solvents, and som

Method used

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Embodiment Construction

[0025] The technical solutions claimed in the present invention will be further described in detail in combination with specific embodiments.

[0026] In the present embodiment, the production technique of sulfachloropyridazine comprises the following steps:

[0027] In a 10L reactor, add 750g of 3,6-dichloropyridazine, 860g of sulfonamide, 1382g of potassium carbonate, and 7.2g of tri-n-propylamine, start stirring, raise the temperature to 140~150°C and keep it warm for 4~5 hours to carry out the condensation reaction . During the condensation reaction, several samples are taken from the reactor and the samples taken out are detected by high performance liquid chromatography. When the mass content of sulfonamide in the material is less than 10%, the condensation reaction is terminated. In other embodiments, the specific amount of each raw material can be adjusted according to the actual situation. In addition, the molar ratio of each should meet the requirements of 3,6-dichl...

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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...

Claims

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Application Information

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IPC IPC(8): C07D237/20G01N30/02G01N30/34G01N30/74G01N30/86
CPCC07D237/20G01N30/02G01N30/74G01N30/34G01N30/8634
Inventor 邱伟杰袁一鸣唐艾臣黄升刘来悦徐伟刘明威
Owner 佛山市南海北沙制药有限公司
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