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Abstract
Monodisperse asymmetrical oligo(phenylene‐ethynylene)s were synthesized iteratively by combining the selective deprotection and the Sonogashira coupling. Trimethylsilylethyl ester (TSE) and trimethylsilyl (TMS) were used as protecting groups for carboxyl and acetylene, respectively. The acetylenic TMS protecting group could be removed selectively by the treatment with TBAF in methylene chloride, whereas both TSE and TMS protecting groups were cleaved in THF.
Acknowledgment
Financial support from CAS (KJCX2‐SW‐H07), the National Natural Science Foundation of China (20225415, 20374053), and the Major State Basic Research Development Program (2002CB613400) are greatly acknowledged.