The phosphinic dipeptides of the general formula H2NCH2CONHCH2P(R)(O)(OH) where R˭Me, Ph and t-Bu has been synthetized from the free phosphinic acids and N-hydroxnunimide esters of the N-protected glycine. The deprotected dipeptida were purified by combination of the column chromato graphy on strong and week cation exchange resins by elution with diluted aqueous ammonia (0.1-3%).