No-Nitrophenylsulfenylamino acid amides of glycine, alanine (DL and L), leucine (DL and L), methionine (DL), phenylalanine (DL and L), and proline (L) were dehydrated in POCl 3- pyridine. The N-protected α-amino-nitriles obtained were treated with anhydrous HCl affording the corresponding α-aminonitrile hydrochlorides. The optical purity of the L-α- aminonitriles was well retained.