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Preparation method of high-purity sulfaquinoxaline

A sulfaquinoxaline and high-purity technology is applied in the field of preparation of high-purity sulfaquinoxaline, can solve the problem of high impurity content of sulfaquinoxaline, and achieves the effects of high product quality, simple preparation process and low impurity content

Pending Publication Date: 2020-05-15
佛山市南海北沙制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sulfaquinoxaline can affect bacterial nuclear protein synthesis, thereby inhibiting the growth and reproduction of bacteria and coccidia. The existing sulfaquinoxaline preparation method is to add gac to remove impurities, and then separate out sulfaquinoxaline crystals with dilute acid water, but When this method removes impurities, because activated carbon cannot remove part of the organic impurities in sulfaquinoxaline, the impurity content of the precipitated sulfaquinoxaline will be relatively high. and the requirements for relevant substances in the 2015 edition of "Chinese Veterinary Pharmacopoeia" are ≤1.0%, so that the current preparation method of sulfaquinoxaline cannot meet today's needs

Method used

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  • Preparation method of high-purity sulfaquinoxaline

Examples

Experimental program
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Effect test

Embodiment 1

[0021] See attached figure 1 , a preparation method of high-purity sulfaquinoxaline, comprising the following steps:

[0022] S1, take by weighing 200 kg of sulfaquinoxaline crude product, 650 liters of water, 1000 liters of ethanol, and 80 kg of industrial liquid caustic soda, then mix and stir the weighed sulfaquinoxaline crude product, water and ethanol and heat up 40 ° C, then Add the weighed industrial liquid caustic soda and mix and stir to dissolve.

[0023] S2, test the pH value of the solution prepared in step S1, if the tested pH value is 10-10.5, then weigh 15 kg of activated carbon, and add activated carbon to the solution prepared in step S1, then heat up to 40 ° C, and finally The solution was decolorized for 25 minutes; if the tested pH value was outside the range of 10-10.5, adjust the pH value of the solution prepared in step S1 to 10-10.5.

[0024] S3. Press filter the solution decolorized in step S2 to separate the filtrate and filter residue, then prepare...

Embodiment 2

[0029] See attached figure 1 , a preparation method of high-purity sulfaquinoxaline, comprising the following steps:

[0030] S1, take respectively 250kg of sulfaquinoxaline crude product, 750 liters of water, 1100 liters of ethanol, and 100kg of industrial liquid caustic soda, then mix and stir the weighed sulfaquinoxaline crude product, water and ethanol and heat up to 45°C, then Add the weighed industrial liquid caustic soda and mix and stir to dissolve.

[0031] S2, test the pH value of the solution prepared in step S1, if the tested pH value is 10-10.5, then weigh 20 kg of activated carbon, and add activated carbon to the solution prepared in step S1, then raise the temperature to 45 ° C, and finally The solution was decolorized for 35 minutes; if the tested pH value was outside the range of 10-10.5, adjust the pH value of the solution prepared in step S1 to 10-10.5.

[0032] S3. Press filter the solution decolorized in step S2 to separate the filtrate and filter residu...

Embodiment 3

[0037] Optimum weighing amount of raw materials:

[0038] See attached figure 1 , a preparation method of high-purity sulfaquinoxaline, comprising the following steps:

[0039] S1, take by weighing 220 kg of sulfaquinoxaline crude product, 720 liters of water, 1080 liters of ethanol, and 90 kg of industrial liquid alkali, then mix and stir the weighed sulfaquinoxaline crude product, water and ethanol and heat up 40 ° C, then Add the weighed industrial liquid caustic soda and mix and stir to dissolve.

[0040] S2, test the pH value of the solution prepared in step S1, if the tested pH value is 10-10.5, then weigh 16 kg of activated carbon, and add activated carbon to the solution prepared in step S1, then heat up to 42.5 ° C, and finally The solution was decolorized for 30 minutes; if the tested pH value was outside the range of 10-10.5, adjust the pH value of the solution prepared in step S1 to 10-10.5.

[0041] S3. Press-filter the solution decolorized in step S2 to separa...

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Abstract

The invention discloses a preparation method of high-purity sulfaquinoxaline. The method comprises the following steps: S1, respectively weighing 200-250 kg of a sulfaquinoxaline crude product, 650-750 liters of water, 1000-1100 liters of ethanol, and 80-100 kg of industrial liquid caustic soda, mixing and stirring weighed sulfaquinoxaline crude product, water and ethanol, heating to 40-45 DEG C,adding weighed industrial liquid caustic soda, mixing, stirring and dissolving. By adding an alcohol organic solvent; organic impurities of sulfaquinoxaline are dissolved; and refining, filtering andseparation are performed to obtain a sulfaquinoxaline refined product with high purity and a low impurity content. The HPLC (High Performance Liquid Chromatography) purity of sulfaquinoxaline can be higher than 99% by the preparation method disclosed by the invention; the content is higher than 99.5%, the impurity content is lower than 0.1%, the requirements, which becomes higher and higher, on veterinary drugs can be met, meanwhile, the whole preparation process is simple, the operation process is simple, the product quality is high, the solvent is convenient to recycle, and the preparation method is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of high-purity sulfaquinoxaline. Background technique [0002] Sulfaquinoxaline belongs to the sulfonamide antibiotics and is used for coccidiosis in livestock and poultry. Sulfaquinoxaline can affect bacterial nuclear protein synthesis, thereby inhibiting the growth and reproduction of bacteria and coccidia. The existing sulfaquinoxaline preparation method is to add gac to remove impurities, and then separate out sulfaquinoxaline crystals with dilute acid water, but When this method removes impurities, because activated carbon cannot remove part of the organic impurities in sulfaquinoxaline, the impurity content of the precipitated sulfaquinoxaline will be relatively high. The higher and higher, and the requirement of relevant substances in the 2015 edition of "Chinese Veterinary Pharmacopoeia" is ≤1.0%, so that the current preparation method of s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/44
CPCC07D241/44
Inventor 黄升黎小雄邱伟杰袁莉莉
Owner 佛山市南海北沙制药有限公司
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