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Preparation method of 3, 5-binitro-2-methyl benzamide

A technology of methyl benzamide and methyl benzoyl chloride, which is applied in 3 fields, can solve the problems of high cost, excess, and ammonia volatilization, and achieve the effects of cost saving, quantitative control, and avoiding volatilization problems

Inactive Publication Date: 2012-07-04
ZHEJIANG RONGYAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional synthesis process of 3,5-dinitro-2-methylbenzamide (commonly known as sclerosin) is to slowly add 3,5-dinitro-2-methylbenzoyl chloride to concentrated ammonia water In the process, stirring and reacting to obtain the finished product of coccolidinone, the disadvantage of this process is that the ammonia water is not easy to quantitatively react, and the amount is too large, resulting in waste of ammonia water and high cost. The environment has brought great harm

Method used

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  • Preparation method of 3, 5-binitro-2-methyl benzamide

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Embodiment 1

[0021] The molar ratio of 3,5-dinitro-2-methylbenzoyl chloride to ammonium chloride is 1:1.

[0022] In a 1000mL four-neck flask equipped with a reflux condenser and a thermometer, add 21.4g of ammonium chloride and 200ml of water, start stirring, and raise the temperature to 35°C within 30 minutes to completely dissolve the ammonium chloride, slowly add 3,5 -Dinitro-2-methylbenzoyl chloride 97.8g, dripped in 1 hour, kept the reaction temperature at 35°C, and continued to react for 2 hours. After the reaction, the reaction solution was filtered, the filter cake was washed with water, filtered, and filtered The cake was dried at 100° C. to obtain 81 g of 3,5-dinitro-2-methylbenzamide (Globalin), with a yield of 90%. The H NMR spectrum is shown in figure 1 shown, and the mass spectrum see figure 2 shown.

Embodiment 2

[0024] The molar ratio of 3,5-dinitro-2-methylbenzoyl chloride to ammonium chloride is 1:3.

[0025] In a 1000mL four-neck flask equipped with a reflux condenser and a thermometer, add 64.2g of ammonium chloride and 600ml of water, start stirring, and raise the temperature to 35°C within 30 minutes to completely dissolve the ammonium chloride, slowly add 3, 97.8g of 5-dinitro-2-methylbenzoyl chloride was dropped in 1 hour, and the reaction temperature was kept at 35°C, and the reaction was continued for 2 hours. After the reaction, the reaction solution was filtered, and the filter cake was washed with water and filtered. The filter cake was dried at 100° C. to obtain 85.5 g of globulin, with a yield of 95%.

Embodiment 3

[0027] Feeding ratio 3, the material ratio of 5-dinitro-2-methylbenzoyl chloride to ammonium chloride is 1:3, and the concentration of ammonium chloride aqueous solution is about 25%.

[0028] In a 1000mL four-neck flask equipped with a reflux condenser and a thermometer, add 64.2g of ammonium chloride and 200ml of water, start stirring, and raise the temperature to 35°C within 30 minutes to completely dissolve the ammonium chloride, slowly add 3, 97.8g of 5-dinitro-2-methylbenzoyl chloride was dropped in 1 hour, and the reaction temperature was kept at 35°C, and the reaction was continued for 2 hours. After the reaction, the reaction solution was filtered, and the filter cake was washed with water and filtered. The filter cake was dried at 100° C. to obtain 89.1 g of globulin, with a yield of 99%.

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Abstract

The invention discloses a preparation method of 3, 5-binitro-2-methyl benzamide, which includes the following steps: 3, 5-binitro-2-methyl benzoyl chloride is slowly and dropwise added to ammonium salt aqueous solution with the mass concentration of 10% to 40%, reaction is conducted for 0.5 hour to 3 hours at the temperature of 10 DEG C to 50 DEG C, after reaction is finished, reaction liquid is filtered, and filter cake is dried to obtain 3, 5-binitro-2-methyl benzamide. The time for dropping 3, 5-binitro-2-methyl benzoyl chloride is 0.5 hour to 3 hours, and the proportion of the amount of 3, 5-binitro-2-methyl benzoyl chloride to the amount of an ammonium salt feeding material is 1:1-6. The preparation method of 3, 5-binitro-2-methyl benzamide uses ammonium salt aqueous solution as an amination reagent, thereby facilitating quantitative control of feeding volume, saving cost, avoiding the problem of ammonia volatilization, and being an environment-friendly, green and efficient synthesis method of Zoalene.

Description

(1) Technical field [0001] The invention relates to a preparation method of 3,5-dinitro-2-methylbenzamide. (2) Background technology [0002] Coccidialin (3,5-dinitro-2-methylbenzamide) is a broad-spectrum, efficient, safe, and residue-free anticoccidiostat, which can promote the growth of chickens when used in feed. It is effective against a variety of Eimeria in chickens, such as tender, poisonous, Brucella, heap-shaped, giant, etc. Eimeria and turkey coccidia. Especially for Eimeria tenabilis and Eimeria poisonous, it mainly inhibits the schizospores of the asexual cycle. The product is not only used for prevention, but also for treatment. The application of treatment dose has no adverse effect on the growth, development and hatching rate of eggs of chickens, and it also has a good effect on the prevention and treatment of coccidiosis in rabbits. [0003] The traditional synthesis process of 3,5-dinitro-2-methylbenzamide (commonly known as sclerosin) is to slowly add 3,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/65C07C231/02
Inventor 石飞吴作鹏詹峰陈仁尔陈建华
Owner ZHEJIANG RONGYAO CHEM
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