微波促进活性炭负载四氯化锡催化合成乙酰乙酸乙酯缩酮

Synthesis of Ketals of Ethyl Acetoacetate Catalyzed by Activated Carbon Supported SnCl_4·5H_2O under Microwave Irradiation

在微波辐射下,以活性炭负载四氯化锡(SnCl4·5H2O/C)为催化剂,不用溶剂,合成了乙酰乙酸乙酯乙二醇缩酮和乙酰乙酸乙酯1,2-丙二醇缩酮。以乙酰乙酸乙酯与乙二醇缩合为模型反应进行优化,其优化条件是:负载量为20%的SnCl4·5H2O/C催化剂0.1 g,乙酰乙酸乙酯5 mL,乙二醇6 mL,微波辐射功率600 W,辐射时间2.5 min,产率达81.6%。产物经过红外光谱表征。

Two ketals were synthesized from ethyl acetoacetate with ethylene glycol and 1,2- propanediol using activated carbon supported SnCl4·5H2O （SnCl4·5H2O/C） as catalysts without solvent under microwave irradiation. Under the optimum reaction conditions （SnCl4·5H2O/C （loaded amount 20%） 0.1 g）, ethyl acetoacetate 5 mL, ethylene glycol 6 mL, microwave power 600 W, microwave irradiation time 2.5 min, the yield of ketal was 81.6%. The products were characterized by IR.