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We report the synthesis of block and alternating thiophene/phenylene co‐oligomers that is based either on the Suzuki coupling reaction or on the Grignard reaction. These reaction schemes enable us to obtain the target compounds at reasonably high yields. The resulting materials have been fully characterized through the solid‐state 13C nmr and Fourier‐transform ir as well as the 1H nmr. Of these, the solid‐state 13C nmr and ir are particularly useful in characterizing the materials of higher molecular weight, since those materials are difficult to dissolve in organic solvents.

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