微波促进活性碳负载单质碘催化合成乙酰乙酸乙酯缩酮

Synthesis of Ketals of Ethyl Acetoacetate Catalyzed by Activated Carbon Supported I_2 under Microwave Irradiation

在微波辐射下,以活性炭负载碘(I2/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。通过改变催化剂负载量、催化剂用量、微波辐射时间、微波辐射功率,研究了这四个因素对乙酰乙酸乙酯缩酮反应收率的影响。以乙酰乙酸乙酯与乙二醇缩合为模型反应进行优化,实验结果表明:I2/C是合成乙酰乙酸乙酯缩酮的良好催化剂,具有良好的催化促进作用。其优化条件是:负载量为10.9%的I2/C催化剂0.07g,乙酰乙酸乙酯5mL,乙二醇6mL,微波辐射功率400W,辐射时间2.5min,产率达100%。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 12 （I2/C） as catalysts without solvent under microwave irradiation .By changing the amount of loaded 12, the amount of catalyst, the microwave irradiation power and the microwave irradiation time,the four factors influencing the yield of the fruetone were studied. Experimental result showed that the catalyst of carbon supported I2 was an excellent catalyst in the synthesis of ethyl aeetoaeetate ketal, has a good catalytic role.Under the optimum reaction conditions （I2/C 0.07 g, loaded amount 10.9%）, ethyl aeetoaeetate 5mL, ethylene glycol 6mL, microwave power 400W, microwave irradiation time 2.5rain, the yield of ketal was 100%.The products were characterized by 1R.