Preparation method of coccidiostat methyl triazon for animal

A technology of methyl triazone and anticoccidia, which is applied in the field of preparation of anticoccidial drug methyl triazone for animals, can solve the problems of low reaction yield, high cost, difficult recovery, etc., and achieves improved The effect of reaction yield

Inactive Publication Date: 2007-03-14
XINFA PHARMA
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Problems solved by technology

[0003] In German patent DE3516631, it is reported that the synthesis of methyl triazone is 1-methyl-5-[3-methyl-4-(4 trifluoromethylthiophenoxy group-)-phenyl]-biuret Prepared by reacting with diethyl carbonate, the reaction yield is low, and the use of diethyl carbonat

Method used

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Example Embodiment

[0016] 1. Preparation of intermediates

[0017] (1) p-Trifluoromethylthiophenol

[0018] 200g of highly active potassium fluoride and 202g of perchloromethanethiol were reacted in sulfolane at 209°C for 1.75 hours, and then reacted at 209-247°C for 3 hours. The reaction product was fractionally distilled to obtain 42 g of trifluorochloromethanethiol.

[0019] Dissolve 18g of phenol and 25g of pyridine in 150ml of chloroform, cool to 0°C, then slowly add 32g of trifluorochloromethanethiol under stirring, and continue stirring for 6 hours after the addition. After the reaction, about 120 ml of chloroform was distilled off. Then 150 ml of diethyl ether was added to the residue, and pyridine hydrochloride was removed by suction filtration. After recovering the solvent, 30.0 g of p-trifluoromethylthiophenol was obtained, with a yield of 72.5% and a purity of 99%.

[0020] (2) Synthesis of 2-methyl-4-nitrochlorobenzene

[0021] Add 1500 ml of hydrochloric acid and 150 g of red ...

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Abstract

The present invention relates to anticoccidial medicine for animal, and is especially preparation process of methyl triazone as one anticoccidial medicine for animal. The preparation process includes the following steps: 1. reacting phenol and trifluoro monochloro methanethiol in the presence of organic base to prepare p-trifluoro methylthio phenol; 2. diazotizing red color base RL and chloric substitution reaction to prepare 2-methyl-4-nitrochlorobenzene; 3. catalytically synthesizing methyl carbamide with urea and methylamine; 4. reacting p-trifluoro methylthio phenol and 2-methyl-4-nitrochlorobenzene to prepare 3-methyl-4-(4- trifluoro methylthio phenoxy)-nitrobenzene; and 5. reducing 3-methyl-4-(4- trifluoro methylthio phenoxy)-nitrobenzene with nitrogen, acylating with nitrogen, condensating, cyclizing and other reaction to prepare final product methyl triazone. The process has low cost and is perfected.

Description

1. Technical field: [0001] The invention relates to an anticoccidial drug for animals, in particular to a preparation method of the anticoccidial drug methyl triazone for animals. 2. Background technology: [0002] Anticoccidial drug for animals 1-[3-methyl-4-(4-trifluoromethylthiophenoxy)-phenyl]-3-methyl-1,3,5-triazine-2,4, The synthetic method of 6 triketone (methyl triazone) has been disclosed in German Patent DE3516630, (1985) and DE3516631 (1985). In German Patent DE3516630, it has been reported that 3-methyl-4-(4-three The synthesis of fluoromethylthiophenoxy)-aniline is to make 3-methyl-4-(4-trifluoromethylthiophenoxy)-nitrobenzene carry out hydrogenation reduction reaction in organic solution, and the catalyst used It is Raney nickel, the reaction pressure is as high as 90-150 atmospheres, and the requirements for reaction equipment are relatively high. [0003] In German patent DE3516631, it is reported that the synthesis of methyl triazone is 1-methyl-5-[3-methy...

Claims

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Application Information

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IPC IPC(8): C07D251/30
Inventor 陈军李新发周正华王涛李涛王举峰
Owner XINFA PHARMA
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