Z-N催化剂内给电子体——9,9-双甲氧基甲基芴的合成研究  

Synthesis of the internal electron donor in Z-N catalyst——9,9-bis(methoxymethyl)fluorene

作　　者：许磊[1] 李效军[1] 刘敏[1] 

机构地区：[1]河北工业大学化工学院,天津300130

出　　处：《化学试剂》2011年第12期1121-1124,共4页Chemical Reagents

摘　　要：以9-芴酮、三甲基碘化亚砜、甲醛水溶液和硫酸二甲酯为主要原料,经Corey-Chaykovsky反应、重排、缩合歧化及醚化反应合成了标题化合物,并对合成反应中的关键影响因素进行了研究。在适宜的反应条件下,目标产物的总收率为68.5%(以9-芴酮计),产品液相色谱纯度为97.4%。通过1HNMR、13CNMR、IR、元素分析和MS对化合物进行了表征,证明产品结构正确。9,9-Bis（methoxymethyl）fluorene was synthesized from 9-fluorenone,trimethylsulfoxoxnium iodide,aqueous formaldehyde and dimethyl sulfate by the Corey-Chaykovsky reaction,rearrangement,condensation/disproportionantion and etherification,the key factors effecting the reactions were studied.Based on the optimized synthetic condition,the overall yield of the desired product was 68.5%,with a purity of 97.4%（analyzed by HPLC）.The structures of the intermediates and the final product were determined by 1HNMR,13CNMR,IR,elemental analysis and MS.

关 键 词：9 9-双甲氧基甲基芴 9 9-双羟甲基芴 9-芴甲醛 9-芴酮 内给电子体 

分 类 号：O625.13[理学—有机化学]