Synthesis of three arms star-shaped poly-b-alanine (3-b-ala) based on tri(prop-2-yn-1-yl) benzene-1,3,5-tricarboxylate (TBT) and azido terminated poly-b-alanine (N 3 -P-ala) was performed using click reaction. TBT was synthesized by nucleophilic substitution reaction between propargyl alcohol and 1,3,5-benzenetricarbonyltrichloride. For the first time, N 3 -P-ala was synthesized through anionic polymerization of acrylamide using sodium azide as an initiator. TBT was characterized by FT-IR and 1 HNMR. N 3 -p-ala was characterized by FT-IR, GPC, and 1 HNMR and 3-b-ala was characterized by FT-IR, GPC, 1 HNMR, TGA, and XRD. The synthesized 3-b-ala was used for drug loading and releasing studies. Polymer loaded drug (3-b-ala-D) hybrid was used in in vitro studies of drug (Diclofenac sodium) release in phosphate buffer solution (PBS) at 37 6 0.5 C and pH 7.4. The drug loading and releasing studies were analyzed by UV-visible spectrophotometer. 3-b-ala-D was examined by AFM to analyze the surface morphology and roughness.