Liu Chun-hong
2010
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Journal
Journal of University of Jinan
Abstract
Through oximating methyl,ethyl and tert-butyl acetoacetates respectively,the effects of oximation agent,solvent and temperature on the cis-trans isomerization of the products were studied.Using sulfuric acid and sodium nitrite as the oximation agent,ethyl acetate and water as the solvent,the optimum temperature range of the reaction for methyl and ethyl acetoacetates was obtained between(15~20)℃.With the same oximation agent,using methyl isobutyl ketone and water as the solvent,the optimum temperature range of the reaction concerning tert-butyl acetoacetate was obtained between(20~25)℃.By high-performance liquid chromatography(HPLC),it was found that the percentage of cis and trans isomers of methyl acetoacetate is 94.5% 3.9%,95.1% 3.4% for ethyl acetoacetate and 92.1% 5.6% for tert-butyl acetoacetate,respectively.