微波辐射活性炭负载杂多酸催化合成乙酰乙酸乙酯缩酮

Synthesis of ketals of ethyl acetoacetate catalyzed by active carbon supported heteropoly acid under microwave irradiation

在微波辐射下,以活性炭负载磷钨酸(HPW/C)和硅钨酸(HSW/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HPW/C催化乙酰乙酸乙酯与乙二醇缩合为模型反应进行优化,优化反应条件:负载量为23 6%的HPW/C催化剂0 4g,乙酰乙酸乙酯10mL,乙二醇10mL,微波辐射功率600W,辐射时间3min,产率达70 7%。产物经过红外光谱表征。

<Abstrcat>Two kinds of ketal were synthesized from ethyl acetoacetate with ethylene glycol and 1,2-propanediol using active carbon supported phosphotungstic acid(HPW/C) and active carbon supported silicotungstic acid(HSW/C) as catalysts and under microwave irradiation.No solvent was used.Under the optimum reaction conditions(HPW/C(loaded amount 23.6 %) (0.4 g), ethyl acetoacetate (10 mL), ethylene glycol (10 mL), microwave power (600 W), microwave irradiation time (3 min)), the yield of ketals was (70.7 %). The products were characterized by IR.