非氧化还原金属离子加速Pd(Ⅱ)催化丁香酚双键异构化反应的研究  

Nonredox metal-ion-accelerated eugenol isomerization and process optimization by palladium(Ⅱ) catalysts

作　　者：何金义 李红静 朱凯[1] HE Jin-yi;LI Hong-jing;ZHU Kai(Chemical Engineering Academy,Nanjing Forestry University,Nanjing 210037,China)

机构地区：[1]南京林业大学化学工程学院,江苏南京210037

出　　处：《应用化工》2018年第3期474-477,共4页Applied Chemical Industry

基　　金：国家自然科学基金(31170536)

摘　　要：以Pd(OAc)_2和Al(OTf)_3为催化剂,研究非氧化还原金属离子加速Pd(Ⅱ)催化丁香酚双键异构化的反应。对不同的非氧化还原金属离子进行筛选,确定选用Al(OTf)_3为非氧化还原金属离子催化剂,采用单因素结合正交实验的方法对丁香酚的双键异构化工艺进行优化。结果表明,最佳工艺条件为:反应温度50℃,反应时间6 h,n[Al(OTf)_3]∶n[Pd(OAc)_2]=2∶1,Pd(OAc)_2和Al(OTf)_3的总用量为3.45%(以丁香酚的质量分数计)。在此条件下,反应稳定性较好,产物得率可达96.3%,其中反式异丁香酚的选择性为89.5%,产品香气较为纯正。采用IR、GC-MS、和~1H NMR等对产物进行了分析与表征。Isomerization of eugenol was investigated by using nonredox metal ion accelerated base to eugenol,Pd(OAc)2 and Al(OTf)3 as catalyst.Different nonredox metal ions were screened,the Al(OTf)3 were determined as nonredox metal ion catalyst and the optimum isomerization conditions based on the orthogonal test results as follow:the reaction temperature is 50℃,the reaction time is 6 h,n[Al(OTf)3]∶n[Pd(OAc)2]=2∶1,the amounts of Pd(OAc)2 and Al(OTf)3 is 3.45%.Three experiment were carried out under these conditions.A good stability was obtained.The yield of the isoeugenol could reach 96.3%with 89.5%selectivity of trans-isomer,and its fragrance was improved greatly.The structure of the product was identified by IR,GC-MS and 1H NMR spectrum.

关 键 词：丁香酚 PD(OAC)2 Al(OTf)3 异构 

分 类 号：TQ654[化学工程—精细化工]