微波辐射下无溶剂催化合成环己酮1,2-丙二醇缩酮

在微波辐射下,以硫酸氢钾为催化剂,不用溶剂,合成了环己酮1,2-丙二醇缩酮。考察了酮醇物质的量比、催化剂用量、微波功率和辐射时间对产品收率的影响。结果表明,硫酸氢钾有着良好的催化活性,在环己酮用量0.2 mol,n(环己酮)∶n(1,2-丙二醇)=1∶1.4,催化剂用量为反应物总质量的1.25%,微波功率450 W,辐射时间10 min条件下,环己酮1,2-丙二醇缩酮收率可达79.2%,催化剂重复使用4次仍保持较高活性。

Catalytic synthesis of cyclohexanone 1,2-propanediol ketal without solvent under microwave irradiation

Cyclohexanone 1,2-propanediol ketal was synthesized from cyclohexanone and 1,2-propanediol using potassium bisulfate as catalyst without solvent under microwave irradiation.The effects of different factors such as molar ratio of reactants,catalyst dosage,microwave irradiation power,microwave irradiation time on the yield of cyclohexanone 1,2-propanediol ketal were carefully investigated.The experimental results showed that potassium bisulfate exhibited excellently catalytic activity.The optimum reaction conditions were as follows:0.2 mol cyclohexanone,molar ratio of cyclohexanone to 1,2-propanediol 1 ∶1.4,1.25% catalyst based on the total mass of the reactants,microwave irradiation power 450 W and irradiation time 10 min.Under these conditions,the yield of cyclohexanone 1,2-propanediol ketal was up to 79.2%.The catalyst could be reused.