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Production Method Of Imazethapyr
Apr 03, 2018

(1) Diketene is treated with chlorine in methylene chloride, ethyl chloroacetoacetate is extracted, and the compound is reacted with methylene chloride at room temperature for 10 hours to obtain 2,4-dichloroacetoacetic acid ethyl ester. Ethyl 2-chloromethyl-ethylnicotinate was prepared by refluxing with 2-ethylacrolein and ammonium sulfamate in anhydrous ethanol for 1.5 hours to prepare 2-amino-2,3-dimethyl Butanamide and sodium bicarbonate were reacted in dimethyl sulfoxide at 80° C. for 6 h. The resulting condensation product was hydrolyzed and then cyclized in acetic acid to obtain imazethapyr.

(2) 2,3-pyridinedicarboxylic acid is reacted with acetic anhydride in toluene to form dipicolinic anhydride, and then reacted with (CH3)2CHCOH3(CN)NH2 at 10-12°C to form carbamoyl nicotinic acid, Hydrogen peroxide was hydrolyzed in an aqueous sodium hydroxide solution, and finally heated to 70° C. to cyclize to obtain imazapyr.

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