Synthesis
Furan-2-carboxylic acid (2.50 g, 22.3 mmol) was used as starting material and dissolved in a solvent mixture of glacial acetic acid (2.0 ml) and carbon tetrachloride (20.0 ml). Bromine (0.8 ml, 13.3 mmol) was added slowly in three portions at 20°C, 6 hours apart, and the reaction was carried out for 5 minutes after addition. The reaction temperature was then maintained at 60°C with continuous stirring for 24 hours. Upon completion of the reaction, the solvent was removed by concentration under reduced pressure. The resulting solid was washed with hot deionized water, filtered and dried to afford 5-bromo-2-furoic acid (3.46 g, 18.1 mmol) in 86% yield.
References
[1] Patent: CN106977476, 2017, A. Location in patent: Paragraph 0073-0093
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[3] Journal of Pharmaceutical Sciences, 1981, vol. 70, # 10, p. 1095 - 1100
[4] Heterocycles, 1994, vol. 38, # 4, p. 759 - 768
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[6] Fakhar U. Zaman, M., Mubarik, A., Kanwal, A., Rasool, N., Ahmad, M., Sohail, M., Malik, A., Al-Hussain, S. A., & Zaki, M. E. A. (2025). Facile Synthesis of 4-(Methoxycarbonyl)phenyl 5-Arylfuran-2-Carboxylates via Readily Available Pd Catalyst–Their Thermodynamic, Spectroscopic Features and Nonlinear Optical Behavior. Catalysts, 15(8), 713.
https://doi.org/10.3390/catal15080713
