Azalactone peptide synthesis is a classical method for the synthesis of dipeptides. Successful synthesis and high yield of dipeptides are the main aim of our study. Valine is an important essential aminoacid of human body, different dipeptide derivative of valine have been synthesized using azalactone peptide synthesis. The UV-Vis, IR, PNMR and Mass spectral studies showed the successful synthesis of dipeptide