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Method for synthesizing fluroxypyr ester

A technology of fluroxypyr ester and a synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of separation, drying, environmental protection problems, long routes, etc., and achieve the effects of improved reaction selectivity, accelerated reaction rate, and convenient operation.

Inactive Publication Date: 2015-05-06
大连科铎环境科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The preparation method of fluroxypyr ester has been studied abroad, mainly by synthesizing sodium pyridinate from 4-amino-3,5-dichloro-2,6-difluoropyridine, and then reacting with 2-octyl chloroacetate to obtain fluorine Grasspyr 2-octyl, or react with methyl chloroacetate, ethyl chloroacetate to synthesize fluroxypyr lower esters, and then obtain fluroxypyr 2-octyl through transesterification, the current method can obtain better reaction yield , but this method has a long route, and there are still problems in separation, drying, environmental protection, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: 100.0 g (0.50 mol) of 4-amino-3,5-dichloro-2,6-difluoropyridine, 62.8 g (0.60 mol) of ethyl glycolate, and 24.0 g of sodium hydroxide were added to 400 g of toluene (0.60mol), raised the temperature to reflux, reacted for 14h, lowered the temperature, washed with water, and post-processed to obtain 112.2g of the product with a yield of 79.3%.

Embodiment 2

[0027] Example 2: 100 g (0.50 mol) of 4-amino-3,5-dichloro-2,6-difluoropyridine, 62.8 g (0.60 mol) of ethyl glycolate, and 82.9 g (0.60 mol) of potassium carbonate were added to 300 g of toluene mol), tetrabutylammonium iodide 1.8g (0.005mol), heated to 100°C, reacted for 10h, added water, thermally separated, the organic phase cooled and crystallized, filtered, and dried to obtain 126.3g of the product, with a yield of 89.2%.

Embodiment 3

[0028] Example 3: 100.0 g (0.50 mol) of 4-amino-3,5-dichloro-2,6-difluoropyridine, 62.8 g (0.60 mol) of ethyl glycolate, and 83.0 g of potassium carbonate ( 0.60mol), tetrabutylammonium bromide 8.1g (0.025mol), heated to 80°C, reacted for 10h, added water, thermally separated, the organic phase cooled and crystallized, filtered, and dried to obtain 127.7g of the product, with a yield of 90.2%.

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PUM

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Abstract

The invention discloses a method for synthesizing fluroxypyr ester. The method comprises the following steps: dissolving 4-amido-3,5-dichloro-2,6 difluoropyridine into a solvent; adding glycollate, an acid-binding agent and a catalyst, heating, and keeping temperature till condensation reaction is complete; and carrying out post-processing to obtain the fluroxypyr ester. The method disclosed by the invention has the beneficial effects of enabling the reaction to be well carried out in a non-polar solvent, namely methylbenzene and the like, by catalyzing the reaction through a phase transfer catalyst, being moderate in condition and wide in application condition, achieving the easiness and convenience for post-processing operation and being simple in route and reduced in cost compared with the traditional process for synthesizing a fluroxypyr ester intermediate.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for synthesizing fluroxypyr ester. Background technique [0002] Fluroxypyr esters include fluroxypyr secondary octyl ester, fluroxypyr methyl ester, fluroxypyr ethyl ester, etc., fluroxypyr methyl ester, fluroxypyr ethyl ester, etc. are used to prepare pesticides: fluroxypyr acid and fluroxypyr secondary An important intermediate of octyl esters. Fluroxypyr sec-octyl ester (1-methylheptyl (4-amino-3,5-dichloro-6-fluoro-2-pyridyloxy) acetate) was developed by Dow Agrochemicals Co., Ltd. The organic heterocyclic herbicide is a fluorine-containing high-efficiency, low-toxicity, and low-residue herbicide. It has the characteristics of high safety for crops in and after crops, wide application period, low dosage, and good compatibility. Has been favored by users. [0003] The preparation method of fluroxypyr ester has been studied abroad, mainly by synthesizing sod...

Claims

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Application Information

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IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 江文书鲁凯李猛李超曹丽贤王善强王乃伟
Owner 大连科铎环境科技有限公司
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