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Method for preparing quinocetone

A kind of quinocetone and catalyst technology, applied in the field of preparation of veterinary drug or aquatic product drug quinocetone, can solve the problems of difficult to form large-scale production, high production cost, environmental pollution, etc., and achieve the requirements of alleviating pollution, low equipment requirements, and reducing production costs. Effect

Inactive Publication Date: 2013-09-11
JINZHOU XINYUAN BIOLOGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because above-mentioned two steps all are condensation reactions, and all adopt catalyst also mostly be inorganic neutral base sodium carbonate or organic strong base triethylamine etc., these bases are accompanied by a large amount of side reactions to take place in the catalytic reaction process, make with benzofuran We calculate that the yield of the first step is lower than 83%, and the yield of the second step is lower than 90% based on the calculation of acemethaquine, so that the total yield of quinocetone target product is very low, only about 75%
In addition, due to a large number of side reactions, there are a large amount of unidentified polymers in the mother liquor after the two-step reaction, which is viscous and difficult to handle, causing great pollution to the environment; and the production cost is higher, and it is difficult to form a large-scale Production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 1000 mL four-neck glass bottle equipped with a stirrer, a thermometer and a condenser, add 137 g (about 1 mol) of benzofurazan and 600 mL of anhydrous methanol. Slowly raise the temperature to 48°C under stirring to completely dissolve the benzofurazan. Then, 102 g (1.02 mol) of 99.8% acetylacetone, 120 g (1 moL) of food grade anhydrous magnesium sulfate and 1 g (0.01 mol) of food grade sodium bicarbonate were added respectively. Slowly raise the temperature to 60°C, make it reflux, and keep it warm for 8 hours, then start sampling and testing. If the reactant benzofurazan is not detected, the surface reaction is complete, and acemethaquine is obtained.

[0024] The reactants in the above-mentioned four-necked glass flask were directly cooled to 30°C, 11g (about 0.1mol) of reagent grade anhydrous sodium carbonate and 112g (1.05mol) of 99.5% benzaldehyde were added, and the temperature was slowly raised to 65°C to allow Reflux, after being incubated for 8 hours, st...

Embodiment 2

[0027] In a 1000 mL four-neck glass bottle equipped with a stirrer, a thermometer and a condenser, add 137 g (about 1 mol) of benzofurazan and 600 mL of anhydrous methanol. Slowly raise the temperature to 48°C with stirring to completely dissolve the benzofurazan. Then, 102 g (1.02 mol) of 99.8% acetylacetone, 111 g (1 mol) of food-grade anhydrous calcium chloride and 1 g (0.01 mol) of food-grade sodium bicarbonate were added respectively. Slowly raise the temperature to 60° C., make it reflux, and keep it warm for 8 hours, then start sampling and testing. If no benzofurazan is detected, it indicates that the reaction is complete and acemetquine has been produced.

[0028] The reactants in the above-mentioned four-necked glass flask were directly cooled to 30°C, 11g (about 0.1mol) of reagent grade anhydrous sodium carbonate and 112g (1.05mol) of 99.5% benzaldehyde were added, and the temperature was slowly raised to 65°C to allow Reflux, after 8 hours of insulation, start sam...

Embodiment 3

[0031] In a 1000 mL four-neck glass bottle equipped with a stirrer, a thermometer and a condenser, add 137 g (about 1 mol) of benzofurazan and 600 mL of anhydrous methanol. Slowly raise the temperature to 48°C under stirring to completely dissolve the benzofurazan. Then, 102 g (1.02 mol) of 99.8% acetylacetone, 111 g (1 mol) of food grade anhydrous calcium chloride and 1 g (0.01 mol) of reagent grade anhydrous sodium carbonate were added respectively. Slowly raise the temperature to 60° C., make it reflux, and keep it warm for 8 hours, then start sampling and testing. If the reaction raw material benzofurazan is not detected, it indicates that the reaction is complete, and acemetquine is obtained.

[0032] The reactants in the above-mentioned four-necked glass flask were directly cooled to 30°C, 11g (about 0.1mol) of reagent grade anhydrous sodium carbonate and 112g (1.05mol) of 99.5% benzaldehyde were added, and the temperature was slowly raised to 65°C to allow Reflux, afte...

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Abstract

The invention relates to a method for preparing quinocetone. The method comprises the following steps of: dissolving benzofuroxan by using methanol and adding diacetone, a catalyst and a dehydrating agent to perform condensation reaction; directly adding benzaldehyde and a catalyst into the reaction mixture; heating to perform the second-step reaction to prepare a quinocetone-containing reaction mixture; filtering the reaction mixture after the second-step reaction; washing by using alcohol and / or washing by using water; and drying under reduced pressure to obtain the quinocetone product. The method is different from the traditional two-step method and the quinocetone product can be directly prepared in the same reaction container, so production cost is reduced and environmental pollution is reduced. In addition, the yield of the quinocetone prepared by the method is over 83 percent and is much higher than the yield, which is 75 percent, of the quinocetone prepared by the traditional preparation method. The product quality meets the standard of the 2003 edition of 'veterinary medicine quality standard' of Department of Agriculture.

Description

technical field [0001] The invention relates to the technical field of veterinary medicine or aquatic product medicine, and more specifically relates to a preparation method of veterinary medicine or aquatic product medicine quinocetone. technical background [0002] Quinocetone (MBQO) is a national first-class new veterinary drug pioneered by Chinese researchers, and its chemical name is 3-methyl-2-cinnamoyl-quinoyl Phenyl-1,4-dioxide, light yellow or yellow-green powder, insoluble in water, slightly soluble in some organic solvents, sensitive to light, prone to photochemical reactions. quinocetone Phenoline drugs have antibacterial, diarrhea-treating, and growth-promoting effects, and have low toxicity and no residue. As a newly developed feed drug additive, quinocetone is used in livestock and poultry, especially young livestock and poultry, which has a significant antibacterial effect in treating diarrhea and promoting growth; it can also be used in aquaculture for a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/52
Inventor 谢文建
Owner JINZHOU XINYUAN BIOLOGY TECH