2,3-Bis(2-cyanoethylthio)-6,7-bis(alkylthio)tetrathiafulvalene derivatives were treated with sodium methoxide to deprotect one 2-cyanoethyl, affording tetrathiafulvalene monothiolate. The generated monothiolate was trapped by 1,4-bis(chloromethyl)benzene to yield the corresponding singly bridged bis- tetrathiafulvalene derivatives. Such derivatives were treated with sodium methoxide again to obtain singly bridged bis-tetrathiafulvalene dithiolate. The dithiolate was reacted with dibromohydrocarbon to afford new type of tetra(tetrathiafulvalene) cyclophanes, and their electrochemical properties and UV spectra were studied by cyclic voltammetry and chemical oxidation, respectively.

Key words: synthesis, cyclic voltammetry, UV spectra, tetra(tetrathiafulvalene) cyclophanes