Purification of Trimetallic Nitride Templated Endohedral Metallofullerenes by a Chemical Reaction of Congeners with Eutectic 9-Methylanthracene

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• 作者：Clairette D. Angeli ; Ting Cai ; James C. Duchamp ; Jonathan E. Reid ; Eric S. Singer ; Harry W. Gibson ; Harry C. Dorn
• 刊名：Chemistry of Materials
• 出版年：2008
• 出版时间：August 12, 2008
• 年：2008
• 卷：20
• 期：15
• 页码：4993-4997
• 全文大小：211K
• 年卷期：v.20,no.15(August 12, 2008)
• ISSN：1520-5002

文摘

The availability of pure samples is a major hurdle in the study of trimetallic nitride templated endohedral metallofullerenes (TNT EMFs). Current HPLC methods of purification are costly, nonrecyclable, and take considerable time. Reported herein is a solvent-free reaction of crude soot extract (empty-cage and Sc or Lu TNT EMFs) in molten 9-methylanthracene that affords almost complete conversion of empty-cage fullerenes to 9-methylanthracene adducts, while leaving TNT EMFs unreacted. After the recovered extract is washed with diethyl ether, the washed extract can then be applied to a silica gel column and subsequently flushed with toluene. To illustrate for Sc₃N@C₈₀, the sample was purified to ∼60% in a time period of <24 h. Final one-step HPLC purification provided high-purity TNT EMF samples (>99%) in an expeditious and less costly manner.