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Solvent-free method for preparing sulfaquinoxaline

A sulfaquinoxaline, solvent-free technology, applied in the field of pharmaceutical technology, can solve problems such as increased production cost, solvent volatilization, environmental pollution, etc., and achieve the effects of eliminating the harm of environmental pollution, improving production yield, and reducing production cost

Pending Publication Date: 2021-01-12
佛山市南海北沙制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional sulfaquinoxaline preparation methods require the use of organic solvents, and the post-production process operations include solvent recovery, purification and other processes, which may cause solvent volatilization, pollute the environment, and increase production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Solventless preparation sulfaquinoxaline method in the present embodiment, comprises the following steps:

[0030] S1. At room temperature, add 220kg of industrial sulfonamide, 190kg of chloride, and 200kg of potassium carbonate into the condensation reactor and stir evenly.

[0031] S2. Raise the temperature of the materials in the condensation reactor to 195~200°C, and keep the system temperature at 195~200°C, and react for 8~9 hours.

[0032] S3. After the reaction is complete, add 1200L of drinking water to the condensation reactor, and stir until the material is completely dissolved.

[0033] S4. Hydraulically feed the material in the condensation reactor to the decolorization reactor.

[0034] S5. Add 20kg of activated carbon into the decolorization reaction kettle, and stir for 8-15 minutes for decolorization.

[0035] S6. Press-filter the materials in the decolorization reaction kettle, and wash the activated carbon in the decolorization reaction kettle with 3...

Embodiment 2

[0045] Solventless preparation sulfaquinoxaline method in the present embodiment, comprises the following steps:

[0046] S1. At room temperature, add 230kg of industrial sulfonamide, 210kg of chloride, and 220kg of potassium carbonate into the condensation reactor and stir evenly.

[0047] S2. Raise the temperature of the materials in the condensation reactor to 195~200°C, and keep the system temperature at 195~200°C, and react for 8~9 hours.

[0048] S3. After the reaction is complete, add 1200L of drinking water to the condensation reactor, and stir until the material is completely dissolved.

[0049] S4. Hydraulically feed the material in the condensation reactor to the decolorization reactor.

[0050] S5. Add 20kg of activated carbon into the decolorization reaction kettle, and stir for 8-15 minutes for decolorization.

[0051] S6. Press-filter the materials in the decolorization reaction kettle, and wash the activated carbon in the decolorization reaction kettle with 3...

Embodiment 3

[0061] Solventless preparation sulfaquinoxaline method in the present embodiment, comprises the following steps:

[0062] S1. At room temperature, add 228kg of industrial sulfonamide, 200kg of chloride, and 210kg of potassium carbonate into the condensation reactor and stir evenly.

[0063] S2. Raise the temperature of the materials in the condensation reactor to 195~200°C, and keep the system temperature at 195~200°C, and react for 8~9 hours.

[0064] S3. After the reaction is complete, add 1200L of drinking water to the condensation reactor, and stir until the material is completely dissolved.

[0065] S4. Hydraulically feed the material in the condensation reactor to the decolorization reactor.

[0066] S5. Add 20kg of activated carbon into the decolorization reaction kettle, and stir for 8-15 minutes for decolorization.

[0067] S6. Press-filter the materials in the decolorization reaction kettle, and wash the activated carbon in the decolorization reaction kettle with 3...

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PUM

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Abstract

The invention discloses a solvent-free method for preparing sulfaquinoxaline, which comprises the following steps: at room temperature, adding industrial sulfanilamide, chloride and potassium carbonate into a condensation reaction kettle, and uniformly stirring; heating the materials in the condensation reaction kettle to 195-200 DEG C, and reacting for 8-9 hours; adding drinking water into the condensation reaction kettle, and stirring until the materials are completely dissolved; pressing into a decoloration reaction kettle; adding activated carbon, stirring and decolorizing for 8-15 minutes; carrying out filter pressing, namely pressing filtrate into a neutralization and crystallization reaction kettle; controlling the material temperature at 80-85 DEG C, dropwise adding a hydrochloricacid solution within 45-60 minutes, and adjusting the pH value to 1.8; slowly stirring and growing crystal for 30 minutes; controlling the temperature of the materials to be 80-85 DEG C, and continuously dropwise adding a hydrochloric acid solution to adjust the pH value to be 1.0; slowly stirring and growing crystal for 60 minutes; discharging, separating crystals and mother liquor, and spin-drying; washing with water, spin-drying, discharging, crushing, and drying at 110-120 DEG C until the water content is less than or equal to 1.0%; and collecting powder to obtain a sulfaquinoxaline dry product.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical technology, in particular to a solvent-free method for preparing sulfaquinoxaline. Background technique [0002] Sulfaquinoxaline is a veterinary API. Conventional sulfaquinoxaline preparation methods require the use of organic solvents, and post-production process operations include solvent recovery, purification and other processes, which may cause solvent volatilization, pollute the environment, and increase production costs. Contents of the invention [0003] The object of the present invention is to overcome the deficiencies in the prior art, provide a kind of technological novelty in the process of preparing sulfaquinoxaline not suitable for organic solvents, reduce solvent volatilization pollution and reduce production cost solvent-free method for preparing sulfaquinoxaline. [0004] In order to achieve the above object, the technical solution adopted in the present invention is: ...

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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