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Preparation method of amitraz

A technology of amitamidine and ethyl formate, applied in the field of compound synthesis, can solve the problems of large amount of three wastes, poor product purity, pollution and the like

Active Publication Date: 2018-03-09
东莞市东阳光动物保健药品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to a series of side reactions, resulting in poor product purity, low yield, and a large amount of three wastes to be treated
The triethyl orthoformate method requires anhydrous conditions, and the reaction needs to be refluxed for a long time, and the introduction of methylamine will take away part of the solvent, resulting in difficulty in recovery and a certain degree of pollution
Monoformamidine, an intermediate of the xylene isocyanate method, is unstable, and the taste of benzene isocyanide is extremely unpleasant, and the whole process is not environmentally friendly.

Method used

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  • Preparation method of amitraz

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preparation example Construction

[0047] The method for preparing amitraz in the above-mentioned embodiments of the present invention mainly uses 2,4-dimethylaniline, N-methylformamide, and triethyl orthoformate as starting materials, and does not use any solvent, and is prepared by a one-pot method. Amitraz. The method has the advantages of environmental protection, high efficiency, economy, short reaction cycle, high product purity and the like.

[0048] The specific reaction equation of the method for preparing amitraz according to the above-mentioned embodiments of the present invention can be expressed as:

[0049]

[0050] According to specific embodiments of the present invention, above-mentioned step (2) is the main step that reacts, specifically carries out according to the following steps:

[0051] (2-1) Heating the mixture to 120 degrees Celsius and controlling the temperature for 1.5-4 hours to generate the compound shown in Formula 1 and volatilize ethanol;

[0052] (2-2) Continue heating the...

Embodiment 1

[0079] The preparation of embodiment 1 amitraz

[0080] In the reaction flask, add 2,4-dimethylaniline (121g, 1mol), N-methylformamide (214g, 1.45mol), triethyl orthoformate (44.2g, 0.75mol), zinc chloride catalyst (1.36g, 0.1mol), 2,4-dimethylaniline hydrochloride catalyst (3.1g, 0.2mol), heating up reaction, when mixture temperature reached 95~96 ℃, began to distill ethanol (due to reaction mass composition Change, the initial temperature of distilling ethanol rises by about 18°C), when the mixture of ethyl formate and ethanol starts to distill out at 135°C, the temperature has been slowly raised to 180°C, the temperature is controlled for 3-7h, and then reduced at -0.07Mpa After reacting for 2 hours, the reaction was monitored by HPLC until the reaction was completed, cooled to room temperature, 200 mL of isopropanol was added and stirred for 1 hour, filtered, and the solid was dried under reduced pressure at 40°C for 5-8 hours to obtain 128 g of amitraz, with a yield of 87...

Embodiment 2

[0081] The preparation of embodiment 2 amitraz

[0082] In the reaction flask, add 2,4-dimethylaniline (121g, 1mol), N-methylformamide (214g, 1.45mol), triethyl orthoformate (44.2g, 0.75mol), zinc chloride catalyst (1.36g, 0.1mol), 2,4-dimethylaniline hydrochloride catalyst (3.1g, 0.2mol), heating up reaction, when mixture temperature reached 95~96 ℃, began to distill ethanol (due to reaction mass composition Change, the initial temperature of distilling ethanol rises by about 18°C), when the mixture of ethyl formate and ethanol starts to distill out at 135°C, the temperature has been slowly raised to 180°C, the temperature is controlled for 3-7h, and then reduced at -0.07Mpa After reacting for 2 hours, HPLC monitored the reaction until the reaction was completed, cooled to room temperature, added 200 mL of ethanol and stirred for 1 hour, filtered, and dried the solid under reduced pressure at 40°C for 5-8 hours to obtain 120 g of amitraz, with a yield of 81.88% and a purity o...

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Abstract

The invention provides a preparation method of amitraz, which comprises the steps of (1) mixing 2,4-methyl toluidine, N-methyl formamide, triethyl orthoformate and a catalyst to obtain a mixture, (2)heating the mixture to allow the mixture to react, and volatilizing alcohol and ethyl formate to obtain final reaction liquid, and (3) cooling the final reaction liquid to a room temperature, and adding an organic solvent for crystallization to obtain the amitraz. The method has the advantages of greenness, environmental protection, high efficiency, economy, short reaction period, high product purity and the like.

Description

technical field [0001] The invention belongs to the field of compound synthesis, in particular, the invention relates to a method for preparing amitraz. Background technique [0002] Amitraz, the common name is Amitraz, the chemical name is N,N-bis(2,4-dimethylphenyliminomethyl)methanamine, and its structural formula is as follows: [0003] [0004] Amitraz is a broad-spectrum acaricide, and also a dual-purpose acaricide for agriculture and animal husbandry. It is an organic nitrogen acaricide with high efficiency and low toxicity, and has a strong contact fumigation effect. In agriculture, it is mainly used for mite damage on fruit trees, vegetables, camellias, cotton, soybeans and other crops, and it also has a good poisonous effect on many other pests. In terms of husbandry, it can treat acarids, bovine mange, bee mites, chiggers and environmental pest mites in cattle, sheep, dogs, pigs and other animals. Amitraz is safe for humans and animals. There is almost no res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/18
CPCC07C257/18
Inventor 雷鑫李东明申燕
Owner 东莞市东阳光动物保健药品有限公司
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