Miao Li
2012
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Journal
Journal of Zhejiang University of Technology
Abstract
Using cyclopropyl methyl ketone,ethyl acetate and phenylguanidine carbonate salt as raw materials,the bactericide Cyprodinil was prepared through the successive reactions of condensation and cyclization.The influences of solvent,temperature,time and molar ratio of materials were investigated.The optimum synthetic conditions were as follows: The condensation reaction solvent was isopropyl ether,n(cyclopropyl methyl ketone)∶n(sodium)∶n(ethyl acetate)=1∶1.3∶1.5,reaction temperature was 65 ℃,reaction time was 3 h.The cyclization reaction solvent reaction was methylbenzene,n(1-cyclopropyl-1,3-butanedione)∶n(phenylguanidine carbonate salt)=1∶0.7,reaction temperature was 110 ℃,reaction time was 3 h.The overall yield of Cyprodinil was 72.4% with the purity of 96.1%.The structures of the product and the intermediate were characterized by 1H NMR and IR.