Lewis酸催化加氢合成天然茴香基丙酮及工艺优化

doi:10.3969/j.issn.0253-2417.2016.03.018

林产化学与工业 ›› 2016, Vol. 36 ›› Issue (3): 121-126.doi: 10.3969/j.issn.0253-2417.2016.03.018

Lewis酸催化加氢合成天然茴香基丙酮及工艺优化

王勇, 吴光耀, 马莉, 朱凯

南京林业大学化学工程学院;江苏省生物质绿色燃料与化学品重点实验室, 江苏南京 210037

收稿日期:2015-04-13 出版日期:2016-06-25 发布日期:2016-07-07
通讯作者: 朱凯,硕士生导师,研究领域为香料香精;E-mail:zhukai53@163.com。 E-mail:zhukai53@163.com
作者简介:王勇(1990-),男,安徽金寨人,硕士生,主要从事香料香精方面研究;E-mail:826109335@qq.com
基金资助:
江苏省高校优势学科建设工程资助项目(无编号)

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

WANG Yong, WU Guang-yao, MA Li, ZHU Kai

Nanjing Forestry University Chemical Engineering Academy;Jiangsu Key Lab. of Biomass-based Green Fuels and Chemicals, Nanjing 210037, China

Received:2015-04-13 Online:2016-06-25 Published:2016-07-07

摘要/Abstract

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。

关键词: 茴香基丙酮, 亚茴香基丙酮, AlCl₃, 加氢

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.

Key words: anisyl acetone, 4-(4-methoxyphenyl)-2-butanone, AlCl₃, hydrogenation

中图分类号:

TQ35

王勇, 吴光耀, 马莉, 朱凯. Lewis酸催化加氢合成天然茴香基丙酮及工艺优化[J]. 林产化学与工业, 2016, 36(3): 121-126.

WANG Yong, WU Guang-yao, MA Li, ZHU Kai. Synthesis and Process Optimization of Hydrogenation of Natural Anisyl Acetone Using Lewis Acid as Catalysts[J]. Chemistry and Industry of Forest Products, 2016, 36(3): 121-126.

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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

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