Abstract: Thiosemicarbazones belong to a large group of thiourea derivatives, which obtained by condensation of thiosemicarbazide with suitable aldehydes or ketones. They have biological activities, such as antitumour, antiviral, anticancer, antifungal, antibacterial and antimalarial. In this work, 4-pyridinecarboxaldehyde thiosemicarbazone was synthesized by the reaction of thiosemicarbazide (TSC) and 4-pyridinecarbaldehyde in 1:1 molar ratio in ethanol under reflux at 70–80 °C for 2 h. The progress of the reaction was monitored by TLC. After the completion of the reaction, a yellow compound was formed, which was characterized by Fourier transform infrared (FT-IR), ¹H-, ¹³C- NMR spectroscopy and elemental analysis. Spectroscopic data: IR (KBr, cm^-1): 3425(s), 3267(s), 3159(s), 1598(s), 1108(s), 829(m), 619(m), 522(m). ¹HNMR (DMSO-d₆, ppm) δH: 7.74(s, 2H), 7.97 (s, 1H ), 8.19 (s, 1H ), 8. 36 (s, 1H), 8.56 (s, 2H), 11.67(s, 1H) ¹³CNMR (DMSO-d₆, ppm) δC: 122.72, 141.13, 143.07, 151.57, 181.