Abstract The application of acetyl chloride in the combination with different solvents and bases permitted the preparation of silyl derivatives of α-and β-cyclodextrines containing a definite amount of acetyl substituents on the secondary hydroxy groups. It was found that by means of the 1 H and 13 C NMR spectroscopy it is possible to make an exact attribution of acetyl groups to C 2 or C 3 carbon atoms of carbohydrate fragments of α-and β- ...