引用本文:
刘长辉, 唐瑞仁, 罗一鸣, 雷存喜. 乙酰丙酮合铜(Ⅱ)催化合成3-氧代-α-紫罗兰酮[J]. 应用化学,
2008, 25(5): 622-625.
Citation: LIU Chang-Hui, TANG Rui-Ren, LUO Yi-Ming, LEI Cun-Xi. Synthesis of 3-oxo-α-Ionone from α-Ionone Oxidized with Oxygen Catalyzed by Cu(acac)2[J]. Chinese Journal of Applied Chemistry, 2008, 25(5): 622-625.
Citation: LIU Chang-Hui, TANG Rui-Ren, LUO Yi-Ming, LEI Cun-Xi. Synthesis of 3-oxo-α-Ionone from α-Ionone Oxidized with Oxygen Catalyzed by Cu(acac)2[J]. Chinese Journal of Applied Chemistry, 2008, 25(5): 622-625.
乙酰丙酮合铜(Ⅱ)催化合成3-氧代-α-紫罗兰酮
摘要:
采用乙酰丙酮合铜(Ⅱ)(Cu(acac)2)催化分子氧氧化α-紫罗兰酮制备了3-氧代-α-紫罗兰酮。采用正交实验考察了制备过程中反应时间、反应温度、催化剂用量、通氧速率、溶剂种类与用量等因素对反应的影响。结果表明,在此催化体系中,α-紫罗兰酮主要发生烯丙位氧化反应生成3-氧代-α-紫罗兰酮,反应温度对反应具有较大的影响。在以质量分数为40%的吡啶作溶剂,使用质量分数为6%的乙酰丙酮合铜(Ⅱ)为催化剂,通氧速率为50 mL/min的条件下,常压80℃时反应10 h,目标产物的收率为40.1%。反应产物的结构经MS、IR、1H NMR及EA等测试技术进行表征。催化剂循环使用5次仍具有较高的催化活性。
English
Synthesis of 3-oxo-α-Ionone from α-Ionone Oxidized with Oxygen Catalyzed by Cu(acac)2
Abstract:
Oxidation of α-ionone catalyzed by Cu(Ⅱ) acetylacetonate (Cu(acac)2) with molecular oxygen as the oxidant was studied.Various factors were investigated including reaction time,reaction temperature,amount of catalyst,oxygen speed,the types and amounts of solvent by using orthogonal test method.The experiment results indicate that reaction temperature affects the reaction significantly,and the yield of the title product was 40.1% when the reaction was run at 80℃ for 10 h with Cu(acac)2 of a mass fraction of 6% as catalyst at an atmospheric oxygen speed of 50 mL/min with pyridine of a mass fraction of 40% as solvent.The structure of product was characterized by MS,IR,1H NMR and elemental analysis.The catalytic activity of Cu (acac)2 was maintained after repeated use for five times.
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Key words:
- allylic oxidation
- / Cu(Ⅱ) acetylacetonate
- / ionone
- / molecular oxygen
- / orthogonal test
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