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) derivatives dithiolate. The dithiolate was reacted with tetra(3'-iodopropythio)- tetrathiafulvalene to afford new type I of pentakis(tetrathiafulvalene) derivatives, and their electrochemical properties and UV spectra were studied by cyclic voltammetry and chemical oxidation, respectively.

Key words: pentakis(tetrathiafulvalene), cyclic voltammetry, UV spectrum, synthesis