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Preparation method of antibacterial veterinary drug sulfamonomethoxine sodium

A technology of sulfamethoxine and sodium metmethoxine, which is applied in the field of preparation of veterinary drug sulfamethoxine sodium, can solve the problems of low yield, cumbersome production process operation, long reaction time, etc., and achieve low cost , The preparation process is simple and the effect of reducing the probability of hydrolysis

Inactive Publication Date: 2017-04-19
杭州洪晟生物技术股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the invention is to solve the veterinary drug sulfamethopyridine sodium for the treatment of animal diseases caused by sensitive bacteria in the prior art. A method for preparing high-purity antibacterial veterinary drug sulfamethopyridine sodium with simple process, high efficiency and high yield

Method used

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  • Preparation method of antibacterial veterinary drug sulfamonomethoxine sodium

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Embodiment 1

[0026] Example 1: (1) Add 12.5g of 4-methoxy-2-aminopyrimidine and 7.9g of anhydrous pyridine into a reactor with a stirring device, heat the temperature to 75°C, and fully stir until 4-methoxy -2-Aminopyrimidine was fully dissolved, and then, under stirring, 0.555 g of anhydrous calcium chloride was added, and then 46.8 g of acetaminobenzenesulfonyl chloride was added to the reactor in batches within 1 hour. , keep the reaction temperature at 75°C, continue the reaction for 4 hours, stop the reaction and filter, pour the crude reaction product into hot water with 4 times the amount of pyridine, stir for 1 hour, refine for 3 hours, filter, wash the filter cake with water until the filtrate is clear, and dry Dry to constant weight to obtain 27.5 g of sulfamethoxine compound with a yield of 98.2% and a purity of 99.5%.

[0027] (2) Dissolve 27.5g of sulfamethoxine in water, heat and stir, heat to 60°C, slowly add 10% sodium hydroxide solution, adjust the pH to 12-13, stir until ...

Embodiment 2

[0028] Example 2: Other reaction conditions remain unchanged, the reaction temperature of step (1) in Example 1 is adjusted to 65°C, and the reaction time is adjusted to 4.5h to obtain 27.4g of sulfamethoxine compound with a yield of 98.0% , with a purity of 99.5%; step (2) with the same reaction conditions, 24.5 g of sulfamethoxine sodium was obtained with a purity of 99.8%.

Embodiment 3

[0029] Example 3: Other reaction conditions remained unchanged, the reaction temperature of step (1) in Example 1 was adjusted to 70°C, and the reaction time was adjusted to 4.5 hours to obtain 27.2 g of sulfamethoxine compound with a purity of 99.1%; Step (2) The reaction conditions were unchanged, and 24.1 g of sulfamethoxine sodium was obtained with a purity of 99.3%.

[0030]Example 3: Other reaction conditions remain unchanged, the amount of the catalyst in step (1) in Example 1 is adjusted to 0.112g, and 26.9g of sulfamethoxine compound is obtained, with a yield of 96% and a purity of 99.0%; Step (2) The reaction conditions were unchanged, and 24.1 g of sulfamethoxine sodium was obtained with a purity of 99.2%.

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Abstract

The invention relates to preparation of a veterinary drug, namely, sulfamonomethoxine sodium used for treating animal diseases caused by sensitive bacteria. An anhydrous lewis acid catalyst, namely, anhydrous calcium chloride is introduced into a condensation reaction step, and 4-methoxy group-2-aminopyrimidine serves as a reaction raw material; in organic alkaline solvent, the 4-methoxy group-2-aminopyrimidine and the catalyst are added in the first place, and then p-acetamidobenzene sulfonyl chloride is added in batches; the effect that moisture in a reaction system is controlled to be always in a low level can be achieved, and meanwhile a reaction substrate can also be effectively activated, so that an intermediate product with the purity being more than 98% can be obtained in short time at a high temperature through a condensation reaction, and the yield can reach more than 95%; and then after hydrolysis, decoloration and crystallization operation in specific mixed crystallization solvent, a target product, namely, the sulfamonomethoxine sodium with the purity reaching more than 99% can be obtained, and the situation of requirements for animal antibacterial veterinary drugs in the prior art is relieved.

Description

technical field [0001] The invention relates to a preparation method of veterinary medicine sulfamethopyridine sodium for treating animal diseases caused by sensitive bacteria. Background technique [0002] Sulfamethopyridine sodium is a long-acting sulfonamide drug. It is a new sulfonamide drug with the strongest antibacterial effect in vivo and in vitro. Its function is to inhibit the growth and reproduction of bacteria mainly through the metabolism of folic acid. It is currently widely used as an antibacterial veterinary drug . It has a significant effect on coccidia, toxoplasma, leucocystosis, etc. Oral administration is well absorbed, the blood concentration is high, and the maintenance time is nearly 24 hours. The acetylation rate is low, the solubility of the acylate is large, it is not easy to cause crystalluria and hematuria, and the curative effect is enhanced when combined with trimethoprim. It is mainly used for the treatment and prevention of respiratory trac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/69
CPCC07D239/69
Inventor 舒建洪张超朱浩艳叶速东赵旭华朱世平
Owner 杭州洪晟生物技术股份有限公司
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