The syntheses of L-α-monomesylin, D-α,β- and DL-α,β-dimesylin, and trimesylin are described and some of their physical properties are reported. It was observed that the optical rotations of L-α-monomesylin and D-α,β-dimesylin in pyridine solutions change with time, whereas the rotations of the same compounds in the sterically hindered base, 2,6-lutidine, remain constant. Of the two previously reported values for the refraction of the –O–SO2– group the value of Tasker and Purves was confirmed. The mono- and dimesylins form the starting materials for the syntheses of the diacyl L-α-monomesylins and the acyl D-α,β-dimesylins.