Silver acetate catalyzed decomposition of the Na-protected a aminodiazoketones in the presence of 'substituted phenol' and triethylamine at - 1s0c lead to 2,4,S-trichlorophenyl esters of Fmoc-/Boc-/Z-J3-homoamino acids in good yield and purity. Thus the homologation of a-amino acids to 13-homoamino acids with concomitant active esters formation has been achieved by this method.