β-环高柠檬醛的合成

Synthesis of β-Cyclohomocitral

以β-紫罗兰酮为原料、50%H2O2为氧化剂合成了β-环高柠檬醛,考察了催化剂种类、催化剂用量、氧化剂用量、反应时间、反应温度等因素对β-环高柠檬醛产率的影响。通过单因素实验确定β-环高柠檬醛的最优合成条件如下:β-紫罗兰酮用量为10.0 g,氧化剂50%H2O2的用量为12 mL,催化剂无水AlCl3的用量为3.0 g,反应时间为8 h,反应温度为45℃。此工艺条件下,β-环高柠檬醛产率可达33.7%。产物结构经GC-MS确证,并用内标法测定其含量。

Using β-ionone as raw material and 50% hydrogen peroxide as oxidant,β-cyclohomocitral was synthesized.The effects of the type and amount of catalyst,the reaction time,the reaction temperature,and the amount of oxidant on β-cyclohomocitral yield were investigated.The optimum reaction conditions were obtained by single factor experiment as follows：for 10.0 g β-ionone,the amount of 50% hydrogen peroxide was 12 mL,the amount of anhydrous aluminum chloride was 3.0 g,the reaction time was 8 h,the reaction temperature was 45℃.Under obove conditions,β-cyclohomocitral yield reached 33.7%.Structure of the product was characterized by GC-MS and its content was determined by internal standard method.