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Finishing treatment method of sulfadoxine

A technology of sulfadoxine and processing method, applied in the field of finishing treatment of sulfadoxine

Pending Publication Date: 2020-01-24
CHANGSHU JINSHEN MEDICAL PROD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Simply using acidic liquid or alkaline liquid adjustment can not really meet the decolorization requirements of higher purity. Therefore, under the discovery of this technology, the applicant hopes to solve this technical problem by seeking a new finishing decolorization treatment method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: add 4500kg water in dissolving pot, add 285kg of sulfadoxine crude product made by CN102391190A embodiment 1 under heating and stirring, add 67.5kg calcium hydroxide to adjust pH value to 12, after fully dissolving, add 22.5kg respectively Activated carbon and 22.5kg of acidic pre-activated pore-expanding activated carbon are used for decolorization, the temperature is at 90°C, and the temperature is kept for 70 minutes; All comparative examples and examples are the same as this implementation condition), centrifugal dehydration; the filter cake is washed with water to clarify the liquid outlet, and the centrifugal drying discharge adopts double cone rotary vacuum drier to dry to obtain the sulfadoxine finished product, which has a purity of 99.95%. %about.

Embodiment 2

[0024] Embodiment 2: add 3600kg water in dissolving pot, add sulfadoxine crude product 261kg that is made by CN102391190A embodiment 2 under heating and stirring, add 45kg calcium hydroxide and adjust pH value to 10.5, after fully dissolving, add 13.5kg gac respectively And 13.5kg of acidic pre-activated pore-expanding activated carbon is used for decolorization, the temperature is 80 ° C, and the temperature is kept for 60 minutes; The liquid port is clarified, and the material is dried by centrifugation in a double-cone rotary vacuum dryer to obtain the finished product of sulfadoxine with a purity of about 99.95%.

Embodiment 3

[0026] Embodiment 3: add 2700kg water in the dissolving pot, add 252kg of the crude product of sulfadoxine obtained by CN102391190A embodiment 3 under heating and stirring, add 22.5kg calcium hydroxide to adjust the pH value to 9.0, after fully dissolving, add 6.75kg respectively Activated carbon and 6.75kg of acidic preactivated pore-expanding activated carbon are used for decolorization, the temperature is 70 ° C, and the temperature is kept for 50 minutes; after cooling, it is filtered by a filter press and sent to a fine crystallization pot for cooling recrystallization and centrifugal dehydration; the filter cake is washed with water until The liquid outlet is clarified, and the material is dried by centrifugal drying with a double-cone rotary vacuum dryer to obtain the finished product of sulfadoxine with a purity of about 99.9%.

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Abstract

The invention discloses a finishing treatment method of sulfadoxine. According to the method, finishing is performed on a crude sulfadimethoxine product generated through a cyclization reaction and achlorination reaction, and an alkaline aqueous solution with a pH value in a range of 8-12.5 is used as a solvent; the crude sulfadimethoxine product is completely dissolved in the alkaline aqueous solution to obtain an alkaline aqueous solution of the crude sulfadimethoxine product, wherein the alkaline aqueous solution of the crude sulfadimethoxine product comprises an impurity A and an impurityB; activated carbon comprises non-pre-activated activated carbon and acidic pre-activated pore-expanded activated carbon, and the acidic pre-activated pore-expanded activated carbon is prepared by soaking activated carbon in an acetic acid or hydrochloric acid solution in advance, carrying out boiling for 2-4 hours and then performing drying before addition into the alkaline aqueous solution of the crude sulfadimethoxine product; and the activated carbon and the acidic pore-expanded activated carbon are added into the alkaline aqueous solution of the crude sulfadimethoxine product at the sametime to decolorize and adsorb impurities in the alkaline aqueous solution of the crude sulfadimethoxine product. According to the invention, a decolorization process is specially designed and improved, so the finishing purity of sulfadoxine can be obviously improved; and the adopted finishing treatment method is simple to operate.

Description

technical field [0001] The invention belongs to the technical field of preparation of sulfonamide antibacterial drugs, in particular to a finishing treatment method of sulfadoxine. Background technique [0002] Sulfadoxine, also known as Zhouxiao sulfonamide, sulfa-o-dimethoxine or 4-sulfa-5,6-dimethoxypyrimidine, is a white or off-white crystalline powder with a slightly bitter taste, odorless, and gradually changes color when exposed to light. Slightly soluble in water, methanol and ethanol, insoluble in ether, soluble in sodium hydroxide and dilute inorganic acids, belonging to sulfonamide antibacterial drugs. Sulfadoxine has the characteristics of long curative effect and low toxicity. It can treat general inflammations, such as upper respiratory tract infection pancreatitis, bacillary dysentery enteritis and skin infections, etc., and it has certain curative effect on the treatment of pulmonary tuberculosis and lymphatic tuberculosis when it is compatible with other dru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/69
CPCC07D239/69
Inventor 李涛徐盛杰
Owner CHANGSHU JINSHEN MEDICAL PROD CO LTD
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