水热驱动的Claisen重排-亲核加成串联反应法合成3-甲基-5-羟基-7-羧基异色满-1-酮  

Synthesis of 3-Methyl-5-Hydroxy-7-Carboxylisochroman-1-One by Cascade Claisen Rearrangement-Nucleophilic Addition Reaction Driven by Hydrothermal Method

作　　者：张广威 胡海慧 李双双[1] 卢文欣 王鹏[1] ZHANG Guang-wei;HU Hai-hui;LI Shuang-shuang;LU Wen-xin;WANG Peng(Chemistry and Biology Engineering College, Shandong University of Science and Technology, Qingdao 266590, China)

机构地区：[1]山东科技大学化学与生物工程学院,山东青岛266590

出　　处：《合成化学》2021年第2期100-104,共5页Chinese Journal of Synthetic Chemistry

基　　金：山东省自然科学基金青年基金资助项目(02011161005)。

摘　　要：研究了基于水热驱动的5-烯丙氧基间苯二甲酸二甲酯的Claisen重排-亲核加成的串联反应,合成了3-甲基-5-羟基-7-羧基异色满-1-酮(K1),其结构经^(1)H NMR,FT-IR和元素分析确证,单晶衍射表征了其晶体结构。通过改变实验条件,获得了原料能够完全转化的临界温度和浓度,分别为120℃和0.02 g/mL。Claisen rearrangement-nucleophilic cascade addition reaction of dimethyl 5-(Allyloxy)isophthalate based on hydrothermal method was studied and the 3-methyl-5-hydroxy-7-carboxylisochroman-1-one(K1).The chemical structure and crystal structure of the product were characterized by ^(1)H NMR,FT-IR,elemental analysis and single crystal diffraction.The optimization conditions which concentration was 0.02 g/mL and under 120℃hydrothermal condition was obtained.

关 键 词：异色满酮 CLAISEN重排 烯丙基芳香醚 水热法 药物中间体 合成 

分 类 号：O621[理学—有机化学]