六甲基萘满的合成优化

Optimization for Synthesis of HMT

采用正交实验设计方法研究了对异丙基甲苯与2,3-二甲基-1-丁烯(2,3-DMB-1)合成六甲基萘满(HMT)的反应。结果表明,该反应较佳的工艺条件为:反应温度20℃,原料摩尔配比2,3-DMB-1:叔丁基氯:对异丙基甲苯:环己烷=1:1.1:1.6:3.4。在此工艺条件下的HMT收率为70%,较文献报道值有明显提高。同时,实验还分析测定了该合成反应的主要副产物,在此基础上对主、副反应的机理进行了推测分析。

1,1,3,4,4,6-hexamethyl-1,2,3,4-tetrahydronaphthalene (HMT), an intermediate for Tonalide, is synthesized from p-cymene and 2,3-dimethyl-l-butene. Based on optimizing synthesis technology route, the optimum conditions of synthesizing HMT were gotten: the temperature 20°C, 2,3-dimethyl-l-butene: tert-butyl chloride: p-cymene: cyclo-hexane = 1:1.1:1.6:3.4. In the optimal condition, the yield of HMT (70.0%) is remarkably higher than that in reference (62.0%). Furthermore, the mechanisms of main and side reactions are speculated based on the analysis of main-product and by-products with GC-MS.