Reducing CO₂ emission is an actual target of research due to its global warming effect. Adsorption of CO₂ by metal-organic frameworks (MOFs) is a promising approach due to their large surface areas, adjustable pore shape, size and properties. One of the most potential strategy to enhance the CO₂ capture capacity of MOFs is the incorporation of functionalities within the pores of MOFs to increase the MOFs?CO₂ interactions. In this work, as an initial step to prepare new functionalized MOFs as adsorbents for CO₂, we design and utilize palladium-catalyzed Sonogashira coupling reactions to synthesize a first organic linker containing both alkyne and nitro functionalities: linker 4-((4-carboxyphenyl)ethynyl)-3-nitrobenzoic acid. Two synthesis routes were investigated and the route using arylacetylenes without nitro group was the route of choice since it gives higher yield of couplings. All obtained compounds included intermediates were characterized by ¹H and ¹³C NMR. The final linker was fully characterized by ¹H, ¹³C NMR, mass and IR spectroscopies.