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以乙酸乙酯和草酸二乙酯为原料 ,经交叉Claisen酯缩合反应合成钠代草酰乙酸乙酯 .讨论反应时间、碱的浓度、原料配比对反应的影响 .得出较佳工艺条件为∶n(乙醇钠 )∶n(乙酸乙酯 )∶n(草酸二乙酯 ) =1 .0 2∶1 .0 2∶1 .0 0 ,乙醇钠浓度为 1 9.5 % ,反应时间为 4h ,产率为 76% .用此盐与苯肼在酸性条件下进行加成缩合反应可制得 1 苯基 3 羧酸乙酯 5 吡唑啉酮 .产物的结构经红外光谱分析确认 .
Ethyl acetate and diethyl oxalate were used as raw materials to synthesize sodium ethyl oxaloacetate by cross-Claisen ester condensation reaction.The effects of reaction time, concentration of alkali and the ratio of raw materials on the reaction were discussed.The optimum technological conditions were as follows: : N (sodium ethoxide): n (ethyl acetate): n (diethyl oxalate) = 1.02: 1 .0 2: 1 0 0, sodium ethoxide concentration 1 9.5%, reaction time 4h, The yield was 76% .Phenyl phenyl 3 carboxylate pyrazolone was obtained by addition condensation reaction of this salt with phenylhydrazine under acidic conditions.The structure of the product was confirmed by IR spectroscopy.