微波辐射氨基磺酸催化合成环己酮1,2-丙二醇缩酮

Synthesis of Cyclohexanone 1,2-Propylene Ketal Catalyzed by Aminosulfonic Acid under Microwave Irradiation

在微波辐射下,以氨基磺酸为催化剂、环己酮和1,2-丙二醇为原料合成环己酮1,2-丙二醇缩酮,研究了反应物摩尔比、微波辐射功率、微波辐射时间、催化剂用量、带水剂用量、反应温度等因素对产品收率的影响。确定最佳反应条件为:环己酮为0.2 mol,n(环己酮)∶n(1,2-丙二醇)=1∶1.3,微波辐射功率500 W,微波辐射时间20 min,催化剂用量为反应物总质量的0.18%,带水剂环己烷用量15 mL,反应温度130℃。在此条件下,环己酮1,2-丙二醇缩酮的收率可达77.2%。

Cyclohexanone 1,2-propylene ketal was synthesized by cyclohexanone and 1,2-propanediol using aminosulfonic acid as catalyst under microwave irradiation. The effects of molar ratio of reactant,microwave irradiation power, microwave irradiation time, catalyst amount, water-carrying agent amount, reaction.temperature on the product yield were discussed. The optimal reaction conditions for 0.2 mol cyclohexanone were obtained as follows.the molar ratio of cyclohexanone to 1,2-propanediol was 1 ： 1.3,the mass ratio of the catalyst to the reactants was 0. 18% ,the microwave irradiation power was 500 W,the microwave irradiation time was 20 min,the water-carrying agent amount was 15 mL,and the reaction temperature was 130℃. Under above conditions, the yield of cyclohexanone 1,2-propylene ketal was 77.2%.