Twonew peptides, a diketopiperazine of Af-methyltyrosine (1) and a tetrapeptide containing N-methyltyrosine (2), were isolated from an actinomycete strain Streptomyces griseus. These compoundsinhibit the enzyme calpain in the micromolar range and were characterized on the basis of spectroscopic analysis, amino acid analysis and sequencing. The structure of the tetrapeptide A^-methyltyrosyl-TV-methyltyrosyl-leucyl-alanine (2), was also confirmed by total synthesis.