Preparation method of mequindox

A technology of acemequine and eggshell, applied in the field of preparation of acemequine, can solve the problems of strong soda ash activity, poor catalytic effect, complicated steps and the like, and achieves the effects of low cost, reduced production process and improved production efficiency

Pending Publication Date: 2022-02-15
BAYECAO HEALTH IND RES INST (XIAMEN) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the oxidation reaction is completed, the synthesis method needs to separate and dry the benzofurazan through post-treatment, and then carry out the next step reaction, the steps are complicated, and the cost is increased; The effect is poor, and the activity of soda ash dissolved is too strong, it is difficult to control

Method used

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  • Preparation method of mequindox
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preparation example Construction

[0024] The invention provides a kind of preparation method of acemetquine, comprising the following steps:

[0025] Mix o-nitroaniline, oxidant, dispersant, catalyst and alcohol solvent for oxidation reaction to obtain benzofurazan product feed liquid;

[0026] Mixing the benzofurazan product liquid and acetylacetone for condensation reaction to obtain acetylmethaquine;

[0027] Wherein, the catalyst is a KOH / eggshell composite; the KOH / eggshell composite includes eggshell powder and KOH loaded on the eggshell powder.

[0028] In the present invention, the synthetic route of described acemetquine is shown in formula A:

[0029]

[0030] The formula A will be specifically described below.

[0031] In the invention, o-nitroaniline, oxidant, dispersant, catalyst and alcohol solvent are mixed for oxidation reaction to obtain benzofurazan product material liquid. In the present invention, the oxidant preferably includes one or more of hydrogen peroxide, sodium hypochlorite, p...

Embodiment 1

[0053] Add 2g of pigeon eggshell powder to 20mL of 3mol / L KOH solution, and stir at room temperature for 1h. Then the solution was filtered, the filtrate was removed, and the powder was dried in an oven at 60° C. for 2 hours to obtain a KOH / eggshell complex.

[0054] Add 5g o-nitroaniline, 40mL ethanol, 1.5g KOH / eggshell complex, 0.25g sodium alginate into the reactor, heat to 30°C, stir until dissolved, then slowly add 5g hydrogen peroxide (mass fraction is 30 %), the temperature was controlled at 30° C., the dropwise addition was completed in 0.5 h, and the reaction was continued for 1 h to obtain the benzofurazan product feed liquid.

[0055] Add 4.8 g of acetylacetone to the benzofurazan product liquid, stir to dissolve, react at 45°C for 8 hours, a yellow solid appears, stop the reaction, place at 4°C for 5 hours, a large amount of solids precipitate out. Filtrate to remove the filtrate, dissolve the solid in acetone (mass volume ratio is 1g:1mL), filter again to remove ...

Embodiment 2

[0058] Add 6g of duck egg shell powder into 60mL of 4mol / L KOH solution, and stir at room temperature for 0.5h. Then the solution was filtered, the filtrate was removed, and the powder was dried in an oven at 60° C. for 1 h to obtain a KOH / eggshell complex.

[0059] Add 10g o-nitroaniline, 80mL ethanol, 4g KOH / eggshell complex, 0.6g sodium carboxymethylcellulose into the reactor, heat to 35°C, stir until dissolved, then slowly add 8g sodium hypochlorite to it, and control the temperature At 35° C., the dropwise addition was completed for 1 h, and the reaction was continued for 1 h to obtain a benzofurazan product liquid.

[0060] Add 11g of acetylacetone to the benzofurazan product liquid, stir to dissolve, react at 50°C for 9h, a yellow solid appears, stop the reaction, place at 4°C for 6h, a large amount of solids are precipitated. Filtrate, remove the filtrate, dissolve the solid in chloroform solution (mass volume ratio is 1g:1mL), filter again, remove the insoluble solid...

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Abstract

The invention relates to the technical field of veterinary drug synthesis, and provides a preparation method of mequindox. According to the invention, o-nitroaniline and acetylacetone are used as raw materials, mequindox is prepared through an oxidation reaction and a condensation reaction, and the oxidation reaction is carried out under the conditions of an oxidizing agent, a dispersing agent and a catalyst; the dispersing agent can make the solution more uniform, and after the oxidation reaction is completed, benzofurazan does not need to be separated, and the next condensation reaction is directly carried out, so production procedures are reduced, and production efficiency is improved; a KOH / eggshell compound is used as the catalyst, KOH is adsorbed in eggshells and can be slowly released in a reaction process, so the KOH has a slow release effect, and the action time of the catalyst is prolonged; and the waste eggshells are used as a catalyst carrier, so a material source is rich, cost is extremely low, and the catalyst is green and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of veterinary drug synthesis, in particular to a preparation method of acemethaquine. Background technique [0002] Acetylmethylquine (Mequnidox, also known as Shibajing, 3-methyl-2-acetylquinoxaline-N-1,4-dioxide), the chemical formula is C 11 h 10 N 2 o 3 , with a molecular weight of 218.21. Acetylmequine is a unique veterinary antibacterial drug in my country. It has broad-spectrum antibacterial properties and is effective against swine dysentery, piglet yellow scour, pullorum, calf paratyphoid, and pullorum And other diseases have good therapeutic effects, and are widely used in veterinary clinics. [0003] At present, the synthetic method of acetylmethaquine mainly is: take o-nitroaniline as raw material, under the effect of alkaline aqueous solution and sodium hypochlorite, ring-forming reaction takes place to obtain benzofuran; benzofuran and acetylacetone, in methanol / ethanol In the solution, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/52B01J23/04B01J27/232B01J32/00
CPCC07D241/52B01J23/04B01J27/232C07B2200/13
Inventor 汤须崇赵应伟熊乐南曹丽平邓爱华
Owner BAYECAO HEALTH IND RES INST (XIAMEN) CO LTD
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