Dilithiation of thiophene (I) employing an excess of BuLi in the presence of TMEDA produced the intermediate 2,5-dilithiothiophene (II). Addition of 4-fluorobenzaldehyde (III) to the organolithium compound (II) afforded the bis-carbinol adduct (IV). Alternatively, addition of benzaldehyde (V) to (II) provided adduct (VI). Boron trifluoride-catalyzed condensation of pyrrole (VII) with diol (IV) yielded the bis(alpha-pyrrolylbenzyl)thiophene (VIII). The dithiaporphyrin derivative (IX) was then obtained by condensation between (VIII) and (VI) in the presence of boron trifluoride. Finally, aromatic sulfonation of (IX) with hot sulfuric acid, followed by neutralization with NaOH furnished the title disulfonate disodium salt.