4,5-环氧-α-紫罗兰酮的合成研究

Synthesis of 4,5-Epoxy-α-Ionone

研究以H2O2为氧化剂,钨酸钠/磷酸/十六烷基氯化吡啶原位合成的过氧钨配合物催化α-紫罗兰酮合成4,5-环氧-α-紫罗兰酮的反应,考察了催化剂用量、反应温度、反应时间、pH值、溶剂及季铵盐等因素对反应的影响。结果表明,以1,2-二氯乙烷作溶剂,nα-紫罗兰酮∶n钨酸钠∶n磷酸∶n十六烷基氯化吡啶∶n过氧化氢=100∶0.3∶0.1∶0.2∶120,pH值为4.0,65℃的条件下反应6h,收率可达85%,其结构通过MS、1H-NMR、IR、EA等检测技术进行表征。

4,5-epoxy-α-ionone was synthesized from α-ionone with hydrogen peroxide as oxidant, and tungsten-based polyoxometallate in-situ synthesized by Na2WO4, H3PO4 and cetylpyridinum chloride （CPC） as catalyst. The influence factors, such as the amount of catalysts, reaction temperature, reaction time, pH values, the kinds of solvents and quaternary ammonium salts were studied. The results showed the yield was 85% under optimum reaction condition as follows： 1,2-dichlorethane as solvent, n（α-ionone） ： n（Na2WO4） ： n（H3PO4） ： n（CPC） ： n（H2O2） = 100 ： 0.3 ： 0.1 ： 0.2 ： 120, the pH value 4, reaction temperature 65℃, reaction time 6 h. The structure was characterized by MS, ^1H-NMR, IR and Element analysis.