Preparation method for sulfadoxine

Abstract

Disclosed is the preparation method for sulfadoxine consisting a condensation reaction and a methyl oxidation reaction, wherein the former consists of charging N,N-dimethyl formamide, sulfonamide sodium salt, chloride into dried reaction container proportionally, then charging sulfonamide sodium salt, solid caustic soda, measuring pH=10, elevating the temperature and measuring pH=10 again, then carrying out in turn heating, heat preservation, recovering, dissolving, diluting, adjusting pH, cooling down, separating, acidifying, adjusting pH, dewatering, scouring and drying.

Description

technical field

[0001] The invention relates to a preparation method of sulfonamide, which is an improvement to the existing preparation method of sulfonamide, and belongs to the technical field of sulfonamide preparation. Background technique

[0002] Zhouxiao sulfonamide (sulfonamide o-dimethoxine) is white or off-white crystalline powder, slightly bitter taste, odorless, gradually changing color when exposed to light, slightly soluble in water, methanol, ethanol, insoluble in ether, soluble in hydroxide Among sodium and dilute inorganic acids, it belongs to sulfa drugs. It can be used to treat pulmonary tuberculosis, lymphatic tuberculosis, malaria, etc., and our country has included it in the "China High-tech Product Export Catalogue" (2003) [7] middle.

[0003] The results of literature search show that: China Zhejiang Yuyao Laike Bioengineering Co., Ltd., China Jiangsu Changshu Jinbai Medical Products Co., Ltd., China Zhejiang Ningbo Jinlu Sprayer Chemical Co., Ltd. ...

Examples

Embodiment

[0013] (1) Put 250Kg N, N-dimethylformamide (DMF) into the dry reaction pot, add 80Kg sulfasulfonamide sodium salt while stirring, and then put in 80Kg 5-methoxyl, which can be made by yourself or purchased commercially. -4,6-dichloropyrimidine, then put in 80Kg sulfonamide sodium salt, and add 10Kg solid alkali, tighten the lid, measure the pH value at 10, naturally heat up to 60°C, then measure pH10, heat up to 90°C , keep warm for 90 minutes, turn on the high-pressure vacuum pump to recover N,N-dimethylformamide (DMF) under reduced pressure, add 300Kg of pure water at 100°C to the recovered 230Kg N,N-dimethylformamide (DMF), and wait until the material After all dissolved, press it into the cooling pot, dilute it with pure water to 1500 liters, adjust the pH to 7.2, then separate the sulfonamide when it is cooled to 15°C, and then rinse it with pure water until the mother liquor reaches 2000 liters, pump it into the precipitation pot, and Acidify with 15% hydrochloric acid ...

technical field

[0001] The invention relates to a preparation method of sulfonamide, which is an improvement to the existing preparation method of sulfonamide, and belongs to the technical field of sulfonamide preparation. Background technique

[0002] Zhouxiao sulfonamide (sulfonamide o-dimethoxine) is white or off-white crystalline powder, slightly bitter taste, odorless, gradually changing color when exposed to light, slightly soluble in water, methanol, ethanol, insoluble in ether, soluble in hydroxide Among sodium and dilute inorganic acids, it belongs to sulfa drugs. It can be used to treat pulmonary tuberculosis, lymphatic tuberculosis, malaria, etc., and our country has included it in the "China High-tech Product Export Catalogue" (2003) [7] middle.

[0003] The results of literature search show that: China Zhejiang Yuyao Laike Bioengineering Co., Ltd., China Jiangsu Changshu Jinbai Medical Products Co., Ltd., China Zhejiang Ningbo Jinlu Sprayer Chemical Co., Ltd. ...

Examples

Embodiment

[0013] (1) Put 250Kg N, N-dimethylformamide (DMF) into the dry reaction pot, add 80Kg sulfasulfonamide sodium salt while stirring, and then put in 80Kg 5-methoxyl, which can be made by yourself or purchased commercially. -4,6-dichloropyrimidine, then put in 80Kg sulfonamide sodium salt, and add 10Kg solid alkali, tighten the lid, measure the pH value at 10, naturally heat up to 60°C, then measure pH10, heat up to 90°C , keep warm for 90 minutes, turn on the high-pressure vacuum pump to recover N,N-dimethylformamide (DMF) under reduced pressure, add 300Kg of pure water at 100°C to the recovered 230Kg N,N-dimethylformamide (DMF), and wait until the material After all dissolved, press it into the cooling pot, dilute it with pure water to 1500 liters, adjust the pH to 7.2, then separate the sulfonamide when it is cooled to 15°C, and then rinse it with pure water until the mother liquor reaches 2000 liters, pump it into the precipitation pot, and Acidify with 15% hydrochloric acid ...