In this chapter, further information about how peptide synthesis is performed, the materials, solid phase peptide synthesis, microwave in peptide synthesis, and the advantages of the microwave are discussed. There are two main peptide synthesization methods: classical solution method and automated solid-phase method. Within these methods, they have their own features and these features have an effect on the peptide synthesis and the peptide yields. Microwave in solid-phase peptide synthesis has many advantages over other methods as they are safer, have higher yields, are faster, etc. Finally, peptide synthesis and characterization methods are explained.