A highly efficient protocol for Arndt-Eistert chain elongation of the
base-labile fluorenylmethoxycarbonyl (Fmoc) protected alpha-amino acid
s by Ag+-catalyzed, ultrasound-promoted Wolff rearrangement of the cor
responding alpha-diazo ketones at room temperature is described. The e
nantiomeric purity of the products was examined by capillary zone elec
trophoresis with chiral buffer systems.