Mono-O-(methylsulfonylethyl)-d-glucoses needed for comparison with the cleavage products obtained by acid hydrolysis of methyl vinyl sulfone modified cotton celluloses have been prepared. Several new glucose derivatives were prepared as intermediates in the synthesis of the desired2-O-, 3-O-, and 6-O-(methylsulfonylethyl)-d-glucoses. The reactions were monitored by gas–liquid chromatography; use was made of trimethylsilyl derivatives as necessary. The substituted glucoses were obtained as glassy solids.