相转移催化法合成异黄樟油素的研究

Study on Synthesizing Isosafrole by Phase Transfer Catalyst

首次将PEG-X和固载PEG-X相转移催化剂用于异黄樟油素的制备,在无溶剂条件下,通过正交实验,得到固载PEG-X催化最优工艺条件为:反应温度90℃,m(黄樟油,88.46%)∶m(KOH)∶m(PEG-X)=1∶0.2∶0.25,反应时间5 h,在此工艺条件下异黄樟油得率为99.89%。固载PEG-X催化剂累计循环使用10次以上,得率未见下降。结果可见:采用相转移固载催化剂PEG-X可提高产品得率,并使异构化温度大大下降。此外,还对黄樟油素重排异构化机理进行了探讨,得出了黄樟油素碱催化的异构化机理。

With PTC PEG- X and Polystyrene supported PTC PEG - X, isosafrole was synthesized in solvent - free conditions from safrole for the first time. The optimal conditions were obtained through orthogonal test. Namely, temperature 90 ℃, m （safrole, 88.46 % ） ： m （KOH） ： m （ PEG - X） = 1 ： 0.2 ： 0.25, time 5 h. Under this conditions, the yields of isosafrole was 99.89 %. Though recycle use of Polystyrene supported PTC PEG- X was more than 10 times, its activity hadn＇t almost declined, the result of test showed that using PTC PEG - X could increase yields of isosafrole and decline temperature of reaction, in addition, the paper put forward base catalysis mechanism by discussing on isomerization mechanism of safrole.