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作 者:张冠群 游翔 霍奕璇 ZHANG Guan-qun;YOU Xiang;HUO Yi-xuan(Anshan Nanjing Cooperation Office,Anshan 114000,Liaoning,China;Anshan Industry Research Institute,Anshan 114000,Liaoning,China)
机构地区:[1]鞍山南京合作办公室,辽宁鞍山114000 [2]鞍山市工业研究院,辽宁鞍山114000
出 处:《香料香精化妆品》2019年第5期13-16,共4页Flavour Fragrance Cosmetics
摘 要:通过对以甲基庚烯酮为原料制备突厥酮的合成工艺进行分析,梳理出试验各步的主要影响因素,根据对比试验确定突厥酮合成反应的最佳条件,即以磷酸为环化剂,三氯甲烷为溶剂,假性突厥酮与磷酸的体积比为1︰4,假性突厥酮与三氯甲烷的体积比为1︰1,反应温度为0℃,反应时间为2 h。从反应过程中发现α-突厥酮的产率比β-突厥酮的产率高,得出本试验优化条件更适宜合成α-突厥酮的结论。试验还从反应的机理、经济性等方面进行了综合考量,对于该工艺路线的优化提升具有重要的参考价值。Based on the analysis of the synthetic process of damascone from methylheptenone, the main influencing factors in each reaction step of the experiment were sorted out. According to the comparative experiment, the optimum conditions for the synthesis of damascone were determined, i.e. phosphoric acid was used as cyclizing agent, trichloromethane was used as solvent, the volume ratio of pseudo-damascone to phosphoric acid was 1/4, the volume ratio of pseudo-damascone to trichloromethane was 1/1, the reaction temperature was 0 ℃, and the reaction time was 2 h. It was found that the yield of α-damascone was higher than that of β-damascone during the reaction. It was concluded that the optimized conditions were more suitable for the synthesis of α-damascone. In addition, the mechanism and economy of the reaction were considered comprehensively, which has important reference value for the optimization and upgrading of the process.
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