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1、AbstractMetamitronisalowtoxicity,highefficiency,lowresidualherbicidewhichiswidelyusedincornfieldsandsugarbeetfields,singleanddoublecotyledonscancontrolweeds.SoMetamitronisimportantherbicideinnthedomesticmarkettheherbicide.1>Ethylbenzoylformatewassynthesizedfromdimethylox
2、alateviathreestepsincludingreplacement,chloridement,Friedel-Craftsreaction.Theprocesswasoptimizedandresultsshowthattheidealreactionconditionsofdiethyloxalylpotassiumarethemolarratio1.06:1(dimethyloxalate:potassiumcarbonate),thereactiontemperature65°C，thereactiontime3h.th
3、eidealreactionconditionsofdiethyloxalylchloridearethemolarratiol:3(threephosgene:diethyloxalylpotassium),thechargingtemperature25°C,thereactiontemperature80°C,thereactiontime5h.theidealreactionconditionsofethylbenzoylformatearethemolarratio1:6(Aluminumtrichloride:benze),
4、thechloridetime3.5h,thereactiontemperature5°C,thereactiontime6h.Comparedwiththereportedroute,theprocessusesalow-costandstablerawmaterialofdiethyloxalate,thetotalyieldwas73.8%andGCpurity99.5%.2、Basisonthereviewofrelevantliteratures,wedevelopedasyntheticrouteofmetamitron.T
5、argetcompundsmetamitronwassynthesizedusinghomemadeethylbenzoylformateasstartingmaterialsinthreestepsincludingaddition,condensationandcyclization.TheproductswerecharacteriedbyIR「HNMRandl3CNMR.Thefactorsofeverystepinprocess,suchasreactiontemperature,reactiontimeandrawmater
6、ialmoleratiowerefoundandoptimized,sotheidealreactionconditionsof2-acetylhydrazinehydrazone-2-phenylethylacetatearethemolarratio1」:1(acetylhydrazine:ethylbenzoylformate),thereactiontemperature70°C,TLCtotrackreactionprocess-theidealreactionconditionsof2-acetylhydrazinehydr
7、azone-2-phenylhydrazineacetylarethemolarratiol:1.5(2-acetylhydrazinehydrazone-2-phenylethylacetate:hydrazinehydrate),thereactiontemperature25°C,thereactiontime24h.theidealreactionconditionsof2-acetylhydrazinehydrazone-2-phenylhydrazineacetylarethemolarratio1:1.5(2-acetyl
8、hydrazinehydrazone-2-phenylethylacetate:hydrazinehydrate),thereactiontemperature25°C,thereactiontime24h
