Abstract
A facile method for the synthesis of (2R,3R)‐1,4‐dimethoxy‐1,1,4,4‐tetrasubstituted‐2,3‐butanediols involving oxidative cleavage of benzylidene acetal as a key step is described. These sterically hindered diols unusually formed cyclic sulfites as the major product under methanesulfonylation reaction conditions.