Preparation of 1-C-glycosyl aldehydes by reductive hydrolysis

► 1-C-Glycosyl aldehydes were prepared by reductive hydrolysis using DIBAL-H. ► Unreported 2-deoxy-glycosyl aldehydes were synthesized. ► Glycopyranosyl aldehydes having 2-alkyloxy group may undergo β-elimination. ► Methyl-protected aldehydes were more stable than benzylated derivatives. ► Sensitive aldehydes can be transformed into stable 1,3-imidazolidine derivatives.