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
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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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