Di‐, tri‐, and tetra‐arginine were prepared from carbobenzoxy‐nitro‐L‐arginine via carbobenzoxy‐nitro‐L‐arginyl‐nitro‐L‐arginine methyl ester, carbobenzoxy‐nitro‐L‐arginyl‐nitro‐L‐arginyl‐nitro‐L‐arginine methyl ester, and carbobenzoxy‐nitro‐L‐argi‐nyl‐nitro‐L‐arginyl‐nitro‐L‐arginyl‐nitro‐L‐arginine methyl ester, respectively, by mixed anhydride and dicyclohexyl‐carbodiimide (DCC) methods. Measurement of the optical rotation of the peptide hydrolysates at 224 mμ showed that no racemization has occurred during the syntheses. Mean residue rotations at 224 mμ of these peptides have some relationship with the chain length. Color values of the Sakaguchi reaction per