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在微波辐射条件下,以绿色溶剂水为溶剂,实现碘催化脱肟反应,以65%~92%的收率获得12种醛酮类羰基化合物。利用核磁共振氢谱(1HNMR)和质谱(MS)对目标产物进行了结构表征。讨论了溶剂的种类、碘的用量、反应温度和微波功率等对反应的影响。确定最优反应条件为:含有不同取代基肟与单质碘摩尔比为n(肟)∶n(碘)=1∶0.5,水为溶剂(肟的浓度为1 mol/L),微波功率为300 W,反应温度为70℃,反应时间为35 min。
Under microwave irradiation conditions, the iodine-catalyzed oxime reaction was achieved with green solvent water as the solvent, and 12 aldehyde and ketone carbonyl compounds were obtained in a yield of 65% -92%. The target product was characterized by 1H-NMR and MS. The effects of solvent type, amount of iodine, reaction temperature and microwave power on the reaction were discussed. The optimal reaction conditions were determined as follows: the mole ratio of oxime to elemental iodine with different substituents was n (oxime): n (iodine) = 1: 0.5, water as solvent (concentration of oxime was 1 mol / L), microwave power was 300 W, the reaction temperature is 70 ℃, the reaction time is 35 min.