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Method for preparing butoxyethyl trichloropyridoxoacetate by aqueous phase synthesis method

A technology of clopyroxyethyl butoxyethyl and pyridyloxy, which is applied in the field of preparation of clopyroxyethyl butoxyethyl by aqueous phase synthesis, which can solve the difficulties of high-quality products and insufficient esterification reaction , affecting product quality and other issues, to achieve clean production, avoid harm to the environment, and achieve the effect of low cost

Inactive Publication Date: 2019-09-06
潍坊新绿化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Triclopyr (triclopyr), as a chloropyridine herbicide, has developed multiple synthetic routes at home and abroad: the original route will produce a large amount of waste water during condensation, and the highly toxic chloroacetic acid is used at the same time. Insufficient esterification leads to low yield. In the final condensation reaction, an isomer is produced which affects product quality. It is difficult to prepare high-quality products with a content of more than 98%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A method for preparing triclopyroxyethyl butoxyethyl ester by an aqueous phase synthesis method, comprising the following steps:

[0018] (1) Add tetrachloropyridine, sodium hydroxide, water and catalyst into the autoclave, raise the temperature in the autoclave to 128°C under stirring, keep the temperature for 1.5 hours, open the autoclave when the temperature drops to 65°C, filter, and wash with appropriate amount of water Filter cake, filter cake drying obtains triclosan sodium;

[0019] (2) Add triclosan sodium, methyl chloroacetate and dimethylformamide to the flask equipped with drier, condenser, thermometer and stirrer, and heat up the reaction system to 60-70°C under stirring, HPLC Track the reaction until the remaining raw material is less than 0.5%, and when the reaction time reaches more than 10 hours, the reaction solution is poured into water, stirred for 2 hours, the product is precipitated, filtered, the filter cake is washed with water, and the filter ca...

Embodiment 2

[0026] A method for preparing triclopyroxyethyl butoxyethyl ester by an aqueous phase synthesis method, comprising the following steps:

[0027] (1) Add tetrachloropyridine, sodium hydroxide, water and catalyst into the autoclave, raise the temperature in the autoclave to 132°C under stirring, keep the temperature for 2.5 hours, open the autoclave when the temperature drops to 75°C, filter, and wash with water Filter cake, filter cake drying obtains triclosan sodium;

[0028] (2) Add triclosan sodium, methyl chloroacetate and dimethylformamide to the flask equipped with drier, condenser, thermometer and stirrer, heat the reaction system to 70°C under stirring, and follow the reaction by HPLC Until the remaining raw material is less than 0.5%, and the reaction time reaches more than 10 hours, pour the reaction solution into water, stir for 2 hours, precipitate the product, filter, wash the filter cake with water, collect and dry the filter cake to obtain 2-(3,5 , 6-trichloro-2...

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PUM

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Abstract

The invention discloses a method for preparing butoxyethyl trichloropyridoxoacetate by an aqueous phase synthesis method, which comprises the following operation steps: (1) adding tetrachloropyridine,sodium hydroxide, water and a catalyst into a high-pressure reaction kettle, carrying out heat preservation reaction, filtering, washing with water, and drying a filter cake to obtain sodium trichloropyridinol; (2) adding sodium trichloropyridinol, methyl chloroacetate and dimethylformamide into a flask provided with a dryer, a condenser, a thermometer and a stirrer, heating the reaction system under stirring, collecting filter cakes and drying to obtain methyl 2-(3,5,6-trichloro-2-pyridyloxy) acetate; (3) adding methyl 2-(3,5,6-trichloro-2-pyridyloxy) acetate, ethylene glycol monobutyl etherand a catalyst into a flask provided with a dryer, a condenser, a thermometer and a stirrer, and obtaining butoxyethyl trichloro-pyridyloxy acetate after reaction treatment. The water phase synthesismethod for preparing the butoxyethyl trichloropyrazolecetate provided by the invention is simple to operate, green and environment-friendly, the starting material is tetrachloropyridine, and the costis lower.

Description

technical field [0001] The technical field of preparation of chemical herbicides of the present invention particularly relates to a method for preparing triclopyroxyethyl butoxyethyl ester by an aqueous phase synthesis method. Background technique [0002] Pyroxypyr (cap irrigation energy), is a systemic conduction selective herbicide, the mechanism of action of synthetic hormones, is not easy to produce resistance, complete control, not easy to relapse, is the world's famous control of trees, shrubs, vines and Agents of malignant broadleaf weeds. This ingredient is absorbed by the leaves and roots of the plant, and is transmitted to the whole plant in the plant, causing deformity of the roots, stems, and leaves, exhaustion of stored substances, embolization or rupture of vascular bundles, and gradual death of the plant. Strong selectivity, highly safe for grass crops. It has special effects on a variety of vicious and difficult-to-control weeds such as chamaejasba, Oxytro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/64
CPCC07D213/64
Inventor 韩超王强姜东升昌胜勇
Owner 潍坊新绿化工有限公司
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