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Lewis酸催化加氢合成天然茴香基丙酮及工艺优化

Synthesis and Process Optimization of Hydrogenation of Natural Anisyl Acetone Using Lewis Acid as Catalysts

  • 摘要: 以天然亚茴香基丙酮为原料,Lewis酸为催化剂,环己烷为氢源,研究了天然茴香基丙酮的合成工艺,并探讨反应机理和反应的选择性。对不同Lewis酸催化剂与溶剂进行筛选,确定AlCl3为催化剂,CH2Cl2为溶剂,采用正交试验方法对茴香基丙酮合成工艺进行优化,得到最佳工艺条件。在反应温度35℃,反应时间4 h, n(AlCl3):n(亚茴香基丙酮)4:1,n(环己烷):n(亚茴香基丙酮)4:1的条件下反应稳定性较好,产物得率达95.1%。采用IR、GC-MS和 1H NMR 等分析技术对合成所得产物进行了表征。

     

    Abstract: Synthesis of natural anisyl acetone was investigated by using natural base to Asia anisyl acetone as raw material, Lewis acid as catalyst, cyclohexane as a source of hydrogen. Different Lewis acid catalysts with different solvents were screened. The optimum synthesis conditions were determined based on the orthogonal test results as follows: the reaction temperature is 35℃, n(AlCl3):n(asia anisyl acetone)4:1 and n(cyclohexane):n(asia anisyl acetone)4:1.Three experiments were carried out under these conditions. A good stability was obtained. The yield of the product 4-(4-methoxyphenyl)-2-butanone could reach 95%. Reaction mechanism and selective of product were discussed. The structure of the product was identified by FT-IR, GC-MS and 1H NMR spectrum.

     

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