Solid-phase synthesis of isomerically pure head-to-tail-coupled (HT) oligo (3- hexylthiophene) s on chloromethylated polystyrene resin has been developed. Using novel sequences of iodination and Suzuki cross-coupling reaction, a series up to a dodecamer has been synthesized in high yield and purity. Removal of the conjugated oligomers from solid support as methyl esters, saponification and decarboxylation to the HT-coupled oligo ...