A Facile and Rapid Route to Highly Enantiopure 1,2‐Diols by Novel Catalytic Asymmetric α‐Aminoxylation of Aldehydes

R- or S-configured 1, 2-diol precursors are formed in good yields (54–86 %) and with excellent enantioselectivities (94 to 99 % ee) by using a simple one-pot sequence—catalytic α-aminoxylation of aldehydes followed by in situ reduction with NaBH4—with L- or D-proline as the catalyst and nitrosobenzene as the oxygen source (see scheme). Supporting information for this article is available on the WWW under http: //www. wiley-vch. de/contents/jc₂002/2003/z52097ₛ. pdf or from the author. Please note: The publisher is not responsible for the content or functionality of any supporting information supplied by the authors. Any queries (other than missing content) should be directed to the corresponding author for the article.