Method utilizing micro-reactor to continuously synthesize amide herbicide

A technology of amide herbicides and microreactors, applied in chemical instruments and methods, preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve the problems of long production cycle, large consumption of lye, low product yield, etc. Achieve the effects of simple production equipment, improved production efficiency, increased yield and product purity

Inactive Publication Date: 2015-01-07
JILIN UNIV
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Problems solved by technology

It overcomes the disadvantages of complex process, long production cycle, large consumpt

Method used

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  • Method utilizing micro-reactor to continuously synthesize amide herbicide
  • Method utilizing micro-reactor to continuously synthesize amide herbicide
  • Method utilizing micro-reactor to continuously synthesize amide herbicide

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Embodiment 1～10

[0031] Inject 2,6-dimethylaniline, chloroacetyl chloride and xylene into micro-reactor 1 with a pore size of 1.5-4 mm through a metering pump for mixed reaction. The reaction temperature is controlled by an external reactor at 50-90 °C, and the reaction stays The time is 6-10 minutes, and the outflowing liquid is chloroacetyl-substituted (2,6-dimethyl)aniline solution.

[0032] Then take the chloroacetyl substituted (2,6-dimethyl) aniline solution, chloromethylene isobutyl ether, and sodium hydroxide solution (50% by mass fraction) prepared by the microreactor 1 and inject the aperture of The mixed reaction is carried out in the microreactor 2 of 0.8-2mm, the reaction temperature is 15-30°C, and the reaction time is 15-40s. Filter the material obtained at the outlet of the microreactor 2, wash the filtrate with an equal volume of water, and recover the solvent under reduced pressure to obtain the finished product of the herbicide ibutachlor. The conversion rate of 2,6-dimethy...

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Abstract

The invention discloses a method utilizing a micro-reactor to continuously synthesize amide herbicide, and belongs to the technical field of organic synthesis. The method takes substituted aniline as the raw material, and then the substituted aniline is subjected to continuous two steps of N-acylation and heterogeneous N-alkylation in a micro-reactor so as to obtain the amide herbicide; wherein the conversion rate of substituted aniline can reach 98% or more, the total yield of the reactions can exceed 95%, and the product purity is more than 96%. The intermediate purifying step is saved, thus the production procedure is simplified, the reaction time is reduced, the alkali solution consumption is reduced, the production equipment is simple, the production efficiency is high, and the product yield and purity are high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for continuously synthesizing amide herbicides by using a microreactor. Background technique [0002] Amide herbicides, mainly including alachlor, acetochlor, metolachlor, pretilachlor, butachlor and isobutachlor, etc., are a class of high-efficiency pre-emergence herbicides, widely used in corn, potato It mainly controls annual grass weeds and various broad-leaved weeds, and has good effect on barnyardgrass, crabgrass, foxtail and millet. [0003] The synthesis of amide herbicides has been reported abroad: mainly including the methylene method (USP 3442945, 3547620, 3630716, 3637847) and the chloroether method (USP 4319917, CN87101526). Due to the relatively low production cost of the chloroether method, it is widely used in the production of amide herbicides. The specific synthetic route is shown in the following formula (taking the synthesis of...

Claims

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Application Information

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IPC IPC(8): C07C231/08C07C233/07
Inventor 张锁秦张广良郑良玉宋善良
Owner JILIN UNIV
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