Synthesis and Characterization of 3,5-Diethoxycarbonyl-2,4-dimethylpyrrole via Knorr Pyrrole Synthesis and its Decarboxylation to 2,4-Dimethylpyrrole: Precursor for Polypyrrole Conductive Polymers for Sodium-Ion Batteries
Year: 2026
Type: dissertation
Abstract: Pyrrole and its derivatives are essential precursors for polypyrrole (PPy), a conductive polymer widely applied in energy storage, corrosion inhibition, and electrochemical sensors. This BSc thesis presents the synthesis of 3,5-diethoxycarbonyl-2,4-dimethylpyrrole via Knorr-type condensation and its subsequent decarboxylation to 2,4-dimethylpyrrole. The synthesis was carried out by nitrosation of ethyl acetoacetate using sodium nitrite, followed by reduction and cyclization with zinc powder at 5-7°C. The crude product yielded 64% with melting point 127-130°C, recrystallized from 95% ethanol to pure pale-yellow crystals (136-137°C). Decarboxylation was achieved via reflux with glacial acetic acid and sulfuric acid, followed by basification and distillation. Product was characterized by FTIR (Agilent Technologies) showing N-H stretch at 3372.84 cm-1, C=O at ~1690 cm-1, C=C at 1659 cm-1, C-N and C-O at 1200-1350 cm-1, confirming formation of substituted pyrrole. This method provides an efficient, low-cost, and reproducible route for substituted pyrrole synthesis, which can be extended to produce various pyrrole derivatives as precursors for conductive PPy-based composites for sodium-ion batteries and energy storage applications. Author: Yusuf Muhammad Ilyasu, Department of pure and Industrial Chemistry, Bayero University Kano, Nigeria. ORCID: 0009-0004-9555-0810. BSc Thesis 2026.
Author: Ilyasu, Yusuf Muhammad
Institution: Bayero University Kano
Language: English
Subfield: Polymers and Plastics
Field: Materials Science
Domain: Physical Sciences
Open Access status: green
OpenAlex ID: W7223288272