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α-蒎烯合成樟脑醌的研究

DOI: 10.3969/j.issn.1000-2006.2013.03.022, PP. 123-128

Keywords: α-蒎烯,2-氯莰烷,冰片烯,樟脑醌

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Abstract:

以α-蒎烯为原料,与hcl加成、异构得到2-氯莰烷,再经消除反应得到冰片烯,以丙酮-水混合溶剂为反应介质,高锰酸钾为氧化剂氧化冰片烯,得到樟脑醌。探讨了相转移催化剂及溶剂种类、kmno4用量、丙酮与水的体积比,以及溶剂用量、反应温度、反应时间等对冰片烯氧化反应的影响,确定了适宜的氧化工艺条件:以高锰酸钾为氧化剂,高锰酸钾与冰片烯的物质量之比为3.0:1;以丙酮-水混合溶剂作为氧化反应介质,丙酮与水的体积比为3:1,丙酮-水混合溶剂与冰片烯的体积质量比为20:1(ml/g);反应温度为30℃;反应时间4h。在此工艺条件下,樟脑醌得率达85%以上。采用gc-ms、ftir、1hnmr、13cnmr等分析手段对合成所得产物的化学结构进行了分析测定。

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