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Preparation method of sulfaclozine sodium

The technology of sulfachlorpyrazine sodium and sulfachlorpyrazine is applied in the field of preparation of sulfa anticoccidial drugs-sulfachlorpyrazine sodium, and can solve the problems of unsatisfactory, difficult to remove and the like

Active Publication Date: 2014-07-02
JIANGSU TIANHE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This impurity is a by-product of condensation reaction, with a content of about 0.6%. It is not easy to remove by the usual 'acid and alkali method'. It cannot meet the requirements of the latest version of the European Pharmacopoeia that the largest single impurity of a medicinal substance is less than 0.2%, and the total impurity is less than 0.5%.

Method used

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  • Preparation method of sulfaclozine sodium

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0018] Example 1: Add 25 grams (0.145 moles) of sulfonamide and 21.6 grams (0.145 moles) of 2,3-dichloropyrazine into a three-necked flask, and dissolve them with 60ml of toluene. Add 22.4 grams of potassium carbonate (0.16 moles) and 2 grams of tetrabutylammonium bromide (0.006 moles) and heat to 110~115°C, keep warm and reflux at 110~115°C for 10 hours, and separate the water at the same time. After the reaction is completed, toluene is recovered under reduced pressure until the reaction temperature reaches 115°C. After the toluene recovery is completed, the temperature of the reaction solution is cooled to 78-82°C, 40 grams of drinking water is added, the pH value is adjusted to 4.5-5.0 with hydrochloric acid, the temperature is lowered to 25°C, filtered and After washing with water, 35.5 g of sulfachlorpyrazine was obtained, with a yield of 86%.

example 2

[0019] Example 2: Add 35 grams (0.2 moles) of sulfonamide and 29.8 grams (0.2 moles) of 2,3-dichloropyrazine into a three-necked flask, and dissolve them with 84 ml of toluene. Add 31.4 grams of potassium carbonate (0.22 moles) and 2.5 grams of benyltriethylammonium chloride (0.011 moles) and heat to 110-115°C, then keep warm and reflux at 110-115°C for 8 hours, while separating the water. After the reaction is completed, toluene is recovered under reduced pressure until the reaction temperature reaches 115°C. After the recovery of toluene is completed, the temperature of the reaction solution is cooled to 80°C. Add 60 grams of drinking water, adjust the pH value to 4.5~5.0 with hydrochloric acid, cool to 25°C, filter and wash with water. Obtain sulfachlorpyrazine 50.3 grams, yield 87%.

[0020] 2. Prepare sulfachlorpyrazine sodium:

[0021] Add 30 grams (0.145 moles) of sulfachlorpyrazine and 120 grams of purified water in a three-necked flask, heat up to 60°C, add 16 gr...

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Abstract

The invention discloses a preparation method of sulfaclozine sodium, belonging to the technical field of chemical synthesis. According to the method, a process condition and a production process are changed, the conventional high-temperature frit reaction between 2,3-dichloropyrazine, sulfanilamide and potassium carbonate is changed, an appropriate solvent is taken as a dissociation agent, an appropriate catalyst is added, the transformation ratio is increased, and the product quality is improved. During refining of a crude product, 'acid and alkali refining' is changed into binary mixed solvent recrystallization, so that the production of a large amount of salt-containing waste water is reduced, and the product purity is increased.

Description

technical field [0001] The invention relates to a preparation method of a sulfonamide anticoccidial drug-sulfachlorpyrazine sodium, which belongs to the technical field of chemical synthesis. Background technique [0002] Sodium sulfachlorpyrazine, chemical name: 4-amino-N-(6-chloro-2-pyrazinyl)benzenesulfonamide sodium monohydrate. White or light yellow powder. This product can compete for dihydrofolate synthase and affect the synthesis of dihydrofolate, thereby inhibiting the growth and reproduction of bacteria and coccidia. The characteristics of this product on poultry coccidia are similar to those of sulfaquinoxaline, but it has stronger antibacterial effect, and can even treat fowl cholera and chicken typhoid, so it is most suitable for the treatment of coccidiosis outbreaks. [0003] The preparation method of existing sulfachloropyrazine sodium, the raw material 2,6-dichloropyrazine and a molecular sulfonamide condensation obtains condensate 2 p-aminobenzenesulfonam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/22A61P33/02
Inventor 王元平
Owner JIANGSU TIANHE PHARMA CO LTD