Two pyridine-2,6-dicarboxylates each containing butynyl and pentynyl at position 2 and 6 were synthesized by esterification of 2,6-pyridinedicarbonyl dichloride with N-alkyne alcohol. All compounds were characterized by using nuclear magnetic resonance spectroscopy (NMR), infrared spectroscopy (IR) and mass spectrometry (MS) techniques. Crystallographic studies showed that both compounds, 3-dibutynyl pyridine-2,6-dicarboxylate (3a) and 4-dipentynyl pyridine-2,6-dicarboxylate (3b) crystallized in monoclinic system with same space group of C 2/c.