活性中间体2,12-二甲氧基-7-氧代-[5]-螺旋烯的合成  

Synthesis and Process Optimization of Active Intermediate 2,12-dimethoxy-7-oxo-[5]-helicenes

作　　者：陈英[1] 张小敏 CHEN Ying;ZHANG Xiaomin(School of chemisty and chemical Engineering,Mianyang Teachers' College,Mianyang,Sichuan 621000)

机构地区：[1]绵阳师范学院化学与化学工程学院,四川绵阳621000

出　　处：《绵阳师范学院学报》2022年第5期39-46,52,共9页Journal of Mianyang Teachers＇ College

摘　　要：7-氧代-[5]-螺旋烯是一种重要的活性中间体,它在材料与催化科学、医药和有机光电等方面都有重要应用.本文以2,7-二羟基萘为原料,经过氧化偶联、醚化、酸催化环化等反应,从克级小试开始摸索反应条件和后处理纯化方法,不断进行工艺优化和放大到百克级合成目标产物,并通过LCMS以及^(1)H NMR对所有中间体和产物进行结构鉴定.7-oxa-[5]-helicenes is an important active intermediate,which has applied in the fields of material,catalytic science,medicine and organic photoelectric and so on.In this paper,2,7-dihydroxynaphthalene was used as raw material,through the reactive processes of oxidation coupling,etherification and acid catalyzed cyclization reactions,the target product was prepared.It also be explored the reaction conditions and purification methods from gram scale validation to scale-up to hundred-gram scale.The structure of all the intermediates and product were determined and characterized by LCMS and ^(1)H NMR.

关 键 词：螺旋烯 联萘 联萘酚 合成 结构表征 

分 类 号：O652[理学—分析化学] O69[理学—化学]