Sulfur containing dextran and beta-cyclodextrin derivatives were synthesised as alternitive coating materials for gold surfaces. The esterification of the carbohydrates with thiophene carboxylic acids and alpha-lipoic acid was carried out in DMSO by in situ activation of the acids with N,N'-carbonyldiimidazole. The thiophene carboxylic acids vary in the position of the sulfur atom and the spacer between the thiophene and the carboxylic group. DS values ranging from 0.44 to 2.04 were accessible depending both on the carbohydrate and the acid used. Insoluble derivatives were obtained by the conversion of a-lipoic acid with the carbohydrates. The structure of the derivatives soluble in DMSO and DMF was examined by IR- and NMR spectroscopy. Furthermore, subsequent acylation reveals a useful tool for the determination of the degree of substitution of the thiophene derivatives additionally to elemental analysis.