Preparation method for preparing sulfonamide sodium salt of sulfadoxine

A technology of sulfadoxine and sulfadoxine sodium, which is applied in the field of preparation of sulfonamide antibacterial drugs, can solve the problems of long preparation cycle, affecting the purity of sulfadoxine, and high energy consumption, so as to reduce energy consumption, ensure product purity, and ensure reaction efficiency Effect

Inactive Publication Date: 2012-07-18
CHANGSHU JINSHEN MEDICAL PROD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Known by the applicant, the preparation of sulfonamide sodium salt by salt-forming reaction in the prior art mainly has the following shortcomings: one, the reaction time is long and causes energy waste, and not only affects production efficiency, but also the sodium content of sulfonamide sodium salt and The nitrogen content is unstable; the second, because the impurity is high and affects the purity of the final sulfadoxine, because the sulfa sodium salt used in the condensation reaction is obtained by the sulfonamide used mechanically, thereby causing the accumulation of impurities, which is finally brought into the terminal The product is sulfadoxine; three, the preparation cycle is long and consumes a lot of energy, because relatively low purity sodium hydroxide is used in the process of preparing sulfa sodium salt, and the water in the reaction process needs to be removed by heating, resulting in lengthy preparation times and reliance on steam heating throughout the process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 25kg of solid sodium hydroxide with a content of 99.5% by weight, 115kg of sulfonamide (industrial grade) (melting point 162-165°C), and 46kg of water into a reaction pot with a stirrer, and heat it under stirring After the solid sodium hydroxide and sulfonamide are all dissolved, continue to heat and distill to remove water, collect dry, and then heat until the material in the pot becomes (in) powder, discharges, and dries to obtain sulfonamide sodium salt, the yield is 135kg, containing Sodium content ≥ 96.5%, nitrogen content ≥ 98.8%. The temperature of the heating, further heating and further heating is all 90°C.

[0023] If the sulfonamide (industrial grade) is replaced by recrystallized sulfonamide, the preparation method of recrystallized sulfonamide is as follows: first put 2000kg of water by weight into a reactor with a stirrer, recover 240kg of sulfonamide, and Heat to 80°C, then use liquid sodium hydroxide to adjust the pH value to 8, dissolve comple...

Embodiment 2

[0025] By weight and content be 22.5kg of solid sodium hydroxide of 99.0%, 80kg of recrystallization sulfonamide, 69kg of water are dropped in the reaction pot, and heating under agitation state, after all dissolvings, continue to heat and distill to remove water and collect dry, and then Heat until the material in the pot becomes powdery, discharge the material, and dry to obtain sulfonamide sodium salt, the yield is 93kg, the sodium content is ≥ 92.5%, and the nitrogen content is ≥ 95.1%. The temperature for said heating, further heating and further heating is 80°C.

[0026] The preparation of the recrystallized sulfonamide is as follows: 2000 kg of water by weight is first dropped into the reactor, and 200 kg of recovered sulfonamide is heated to 100° C. under stirring, and the pH value is adjusted to 7 with liquid sodium hydroxide. Dissolve completely at 100°C, add activated carbon to keep warm for decolorization, continue to filter while hot, cool to crystallize, cent...

Embodiment 3

[0028] 20kg of solid sodium hydroxide with a content of 98.5% by weight, 150kg of sulfonamide or recrystallized sulfonamide, and 92kg of water are put into the reaction pot, and heated under stirring, continue to heat after dissolving, distill and remove water to dry up, Then heat until the material in the pot becomes powdery, and dry the material to obtain sulfonamide sodium salt, the yield is 180kg, the sodium content is ≥ 91.5%, and the nitrogen content is ≥ 95.0%. The temperature of the heating, further heating and further heating is 100°C.

[0029] The preparation of the recrystallized sulfonamide is as follows: 3000 kg of water by weight is first dropped into the reactor, and 120 kg of recovered sulfonamide is heated to 90°C under stirring, and the pH value is adjusted to 6 with liquid sodium hydroxide. Dissolve completely at 90°C, add activated carbon to keep warm for decolorization, continue to filter while hot, cool to crystallize, centrifugally filter at 30°C, wa...

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Abstract

The invention discloses a preparation method for preparing a sulfonamide sodium salt of sulfadoxine, belonging to the technical field of preparation of a sulfonamide antibacterial medicament. The method comprises the following steps of: putting solid sodium hydrate, technical grade sulfonamide or recrystallized sulfonamide and water into a reaction pot with a stirrer; heating and dissolving in a stirring state; after the solid sodium hydrate and the recrystallized sulfonamide are fully dissolved, continually heating and carying out distilling for removing water to dryness; further heating till materials in the reaction pot become powder; and discharging and drying to obtain the sulfonamide sodium salt of which the sodium content is more than or equal to 90 percent and the nitrogen content is more than or equal to 92 percent. The method has the advantages that: the sodium content and the nitrogen content of the obtained sulfonamide sodium salt are stable; the quality of the sulfonamide sodium salt can be guaranteed, the reaction efficiency of a next procedure is ensured, and impurities in a finished product are reduced; impurities brought into the finished product can be reduced, and the product purity is ensured; and a final finished product, i.e. sulfadoxine, prepared from the sulfonamide sodium salt obtained by the method has high purity.

Description

technical field [0001] The invention belongs to the technical field of preparation of sulfonamide antibacterial drugs, in particular to a method for preparing sulfadoxine sodium sulfonamide salt. Background technique [0002] The chemical name of sulfadoxine (SDM) is: 4-(p-aminosulfonamide) 5,6-dimethoxypyrimidine; the English name is: Sulfadoxine; the Latin name is: Sulphamethoxinum or Sulfadimoxine; the molecular formula is C 12 h 14 o 4 N 4 S; molecular weight 310.33. [0003] 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,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/38C07C303/40
Inventor 李涛
Owner CHANGSHU JINSHEN MEDICAL PROD CO LTD
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