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芳炔在矽誘導菲合成以及「一瓶化」的咪唑烷合成中之應用
Dissertation

芳炔在矽誘導菲合成以及「一瓶化」的咪唑烷合成中之應用

Sharada Prasanna Swain
Doctor of Philosophy (PHD), 國立清華大學, 化學系
2012

Abstract

芳炔 船舶基地 1,3 - 偶极环加成 咪唑 Aryne Silicon Phenanthrene Schiff base 1,3-Dipolar cycloaddition Imidazolidine
Arynes are highly reactive intermediates which possess numerous applications in organic synthesis. Arynes have been used in several transition metal-catalyzed reactions. Recently, efforts have been devoted to transition metal free reactions, which include the initial addition of nucleophiles to arynes and subsequent trapping with electrophiles. In this thesis, I reported a new method for the synthesis of (-phenanthrenyl)vinylsilanes from benzynes and allenylsilanes. Compounds containing phenanthrene moiety possess luminescence and fluorescence properties. Attachment of a silyl group directly to allenes allowed their reactions with substituted benzynes at 0 °C to produce (-phenanthrenyl)vinylsilanes exclusively in 66–92% yields through a [2 + 2 + 2] pathway. Without a silyl group in allenes, the reaction proceeded by entirely different pathways to give a mixture. These results indicate the existence of an unprecedented silicon-induced arene formation, of which mechanism and generality are discussed. To continue the study of transition metal free reactions involving arynes, I utilized these reactive intermediates arynes to develop a new aryne-induced reaction. I developed a new method for the synthesis of imidazolidines, a class of compounds with biological activities of value. By use of the 1,3-dipolar cycloaddition strategy, a Schiff base bearing an ester or a cyano group at the  carbon atom was arylated with an aryne that were generated from (trimethylsilyl)aryl triflates and cesium fluoride. Then an intramolecular proton transfer took place from the  position to the anionic aryne ring to give an azomethine ylide. This ylide reacted with a second equivalent of the same Schiff base in situ at 25 °C through a [3 + 2] fashion to produce the desired imidazolidines in 70–85%. This “one-flask” method proceeded with very high stereoselectivity that all of three substituents attached to the carbon atoms in the imidazolidine ring held in cis configuration. This is the first aryne-induced cyclization reported in the synthesis of five-membered heterocycles.

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