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Method for synthesizing pretilachlor

A synthetic method and technology of pretilachlor, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., can solve the problems of low process yield, high cost of raw materials, high synthesis cost, etc., and achieve low toxicity of reagents , the number of solvents is small, and the effect of equipment corrosion is small

Inactive Publication Date: 2011-11-02
NANTONG WEILIKE CHEM
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Problems solved by technology

[0004] Based on the above two synthetic methods, method 1) is relatively simpler than method 2), but method 1) the process yield of the final step of the synthetic product is too low, making its synthesis cost relatively high, while synthetic method 2) is relatively simple to operate. complex, and the cost of raw materials used is also high, therefore, there is an urgent need for a synthetic method with high economic efficiency, good yield, few side reactions and environmental friendliness to promote the application and production of this kind of pesticide

Method used

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  • Method for synthesizing pretilachlor
  • Method for synthesizing pretilachlor
  • Method for synthesizing pretilachlor

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Embodiment 1

[0020] Embodiment 1: the preparation of pretilachlor.

[0021] 1) Synthesis of N-(1-methyl-2-hydroxyethyl)-2,6-diethylaniline: in a 500ml four-necked flask, equipped with electric stirring and a thermometer, add 2,6-diethylaniline ( 14.9g, 0.2mol), 0.2g of zinc chloride, 1ml of glacial acetic acid, 150ml of water, 150ml of methanol, start stirring, keep the temperature at 10-15°C, slowly introduce ethylene oxide gas, and keep it until the gas does not overflow. , and weighed at all times. After the system gained 9g in weight, stop ventilation, return to room temperature and stir for 2h. After the reaction, methanol was distilled off, separated and washed with water to obtain 23.3g of oily substance, with a yield of 95%. The target product was detected by NMR.

[0022] (2) Synthesis of 2-ethyl-6-methyl-N-(1'-methoxy-prop-2-yl) aniline: in a 500ml three-necked flask, an electric stirrer, a thermometer, a reflux condenser, and N -(1-methyl-2-hydroxyethyl)-2,6-diethylaniline (39...

Embodiment 2

[0025] Embodiment 2: the preparation of pretilachlor.

[0026] 1) Synthesis of N-(1-methyl-2-hydroxyethyl)-2,6-diethylaniline:

[0027] In a 500ml four-neck flask, equipped with electric stirring and a thermometer, add 2,6-diethylaniline (14.9g, 0.2mol), 0.3g of zinc acetate, 1ml of glacial acetic acid, 200ml of ethanol, start stirring, and keep the temperature at 20°C Left and right, slowly feed ethylene oxide gas, keep the gas not overflowing, and weigh it all the time. After the system has gained 9g in weight, stop the ventilation, return to room temperature and stir for 2 hours. Obtained 23.6 g of oily substance, yield: 96%. The target product was detected by NMR.

[0028] 2) Synthesis of 2-ethyl-6-methyl-N-(1'-methoxy-prop-2-yl)aniline:

[0029] In a 500ml three-necked flask equipped with an electric stirrer, a thermometer, and a reflux condenser, add N-(1-methyl-2-hydroxyethyl)-2,6-diethylaniline (39.4g, 0.2mol), normal chlorine Propane 300ml, concentration is 80% so...

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Abstract

The invention discloses a method for synthesizing pretilachlor. The method for synthesizing the pretilachlor sequentially comprises the following steps of: synthesizing N-(1-methyl-2-hydroxy ethyl)-2,6-diethylaminobenzene; synthesizing 2-ethyl-6-methyl-N-(1'-methoxyl-propyl-2-group)phenylamine; and synthesizing the pretilachlor and the like. The method is simple and practical and high in efficiency; yield of products in each step is over 92 percent; in the synthetic process, the adopted reagent has low toxicity, few solvents are used and few side reactions are generated, so corrosivity to equipment is low and environmental friendliness is achieved; and the raw materials are low in price, so the production cost is reduced, economical efficiency is high, and a good application prospect is achieved.

Description

technical field [0001] The invention belongs to the field of agricultural herbicides, in particular to a method for synthesizing pretilachlor. Background technique [0002] Since herbicides and other insecticides and fungicides have similar application effects, organisms such as weeds and pests will develop resistance to their effects when used for a long time. Therefore, it is necessary to continuously invent new compounds with different effects and have It is a new variety that can be mass-produced industrially, and pretilachlor pesticide meets the above various requirements, and has already produced a large amount in the industry, and has received widespread attention in the market. [0003] Pretilachlor is a special herbicide for paddy fields with high selectivity and broad herbicidal spectrum. It is safe to rice, and this product is a pre-emergence herbicide, mainly used to control grass weeds, belonging to 2-chlorinated acetanilide herbicides, is a cell division inhib...

Claims

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Application Information

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IPC IPC(8): C07C233/88C07C213/02
Inventor 李可庆蒋慧华章奉良
Owner NANTONG WEILIKE CHEM
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