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合成了大环双核铜(Ⅱ)催化剂—{[Cu(Ⅱ)aneN5]2(DDS)}(ClO4)4,用元素分析和红外光谱对其结构进行了表征。常压条件下,以制得的催化剂催化分子氧氧化环己烯合成环己烯酮,考察了催化剂用量、反应时间、反应温度、溶剂用量等因素对环己烯酮合成的影响。优化得到较佳合成工艺条件为:O2流速大约5 mL/min,以环己烯4 mL计,催化剂2 mg,反应时间12 h,反应温度338 K,乙腈12 mL。环己烯的转化率为65.9%,环己烯酮的选择性为78.3%。
The macrocyclic binuclear copper (Ⅱ) catalyst - {[Cu (Ⅱ) aneN5] 2 (DDS)} (ClO4) 4 was synthesized and its structure was characterized by elemental analysis and infrared spectroscopy. Under normal pressure, cyclohexene oxide was synthesized by the molecular oxygenation of cyclohexene catalyzed by the obtained catalyst. The effects of the amount of catalyst, reaction time, reaction temperature and the amount of solvent on the synthesis of cyclohexenone were investigated. The optimized synthesis conditions were: O2 flow rate was about 5 mL / min, cyclohexene 4 mL, catalyst 2 mg, reaction time 12 h, reaction temperature 338 K and acetonitrile 12 mL. The conversion of cyclohexene was 65.9%, and the selectivity of cyclohexenone was 78.3%.