Abstract: With microwave radiation,ethyl acetoacetate glycol ketal was synthesized from ethyl acetoacetate and glycol using acid-treated Al-crosslinked montmorillonite as catalyst without solvent.The effects of catalyst dosage,reaction temperature,molar ratio of reactants,microwave irradiation time and power on the yield of the ketal were investigated.The optimum reaction conditions are as follows:the quantity of catalyst in material is 3%,the reaction temperature is 100 ℃,reaction time is 5 min,molar ratio of ketone to alcoholic is 1.0∶1.2,and microwave radiate power is 500 W,the yield of the ketal is about 71.9%.The reaction speed of microwave calefaction method is about 18 times higher than general calefaction method.

Key words: Microwave radiation, Montmorillonite, Fructone

摘要： 对微波辐射条件下,酸化铝交联蒙脱土为催化剂,无溶剂条件下合成乙酰乙酸乙酯乙二醇缩酮进行了研究。研究了催化剂用量、反应温度、反应物投料比、微波辐射时间和功率对缩酮收率的影响,并与常规加热法进行了对比。结果表明,催化剂质量分数为3%,反应温度100℃,反应时间5min,酮醇物质的量比1.0∶1.2,辐射功率500W 时,缩酮收率可达71.9%。达到相同转化率,微波法反应速率是常规加热法的18倍。

关键词: 微波辐射, 蒙脱土, 苹果酯