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在无溶剂条件下,以SO_(42)-/TiO_2-SnO_2固体超强酸为催化剂,合成了季戊四醇双缩苯乙酮,考察了催化剂的用量、反应物的摩尔比、反应时间和反应温度等对缩酮反应的影响。结果表明,催化剂的用量为反应物总质量的1.6%,季戊四醇和苯乙酮的摩尔比为1:2.2,反应温度为175℃,反应时间为4 h时,季戊四醇双缩苯乙酮的产率达98.6%。对产物进行了1HNMR、MS、单晶衍射表征。该方法具有合成工艺简单、温度可控、产率高、产物易于分离、不产生污染、催化剂可重复使用等优点,具有良好的工业应用前景。
In solvent-free conditions, pentaerythritol bisacetophenone was synthesized using SO42- / TiO2-SnO2 solid superacid as catalyst, and the effects of the amount of catalyst, molar ratio of reactants, reaction time and reaction temperature Effect of ketal reaction. The results showed that the yield of pentaerythritol diacetophenone was 1.6% of the total mass of the reactants, the molar ratio of pentaerythritol to acetophenone was 1: 2.2, the reaction temperature was 175 ℃ and the reaction time was 4 h. Up to 98.6%. The product was characterized by 1HNMR, MS and single crystal diffraction. The method has the advantages of simple synthesis process, controlled temperature, high yield, easy product separation, no pollution and reusable catalyst, and has good industrial application prospect.