TY - JOUR
T1 - Fe-phosphomolybdic acid/mesoporous SiO2
T2 - A Highly efficient catalyst for the synthesis of Medicinally important organic compounds
AU - Abo El-Yazeed, Wafaa S.
AU - El-Hakam, S. A.
AU - Kospa, Doaa A.
AU - Hayes, O. R.
AU - Khder, A. S.
AU - Ibrahim, Amr Awad
AU - Ahmed, Awad I.
N1 - Publisher Copyright:
© 2025 Elsevier B.V.
PY - 2025/4
Y1 - 2025/4
N2 - In this study, we synthesized Fe-exchanged phosphomolybdic acid catalysts supported by mesoporous SiO2 (FePMA/mSiO2) using an ion-exchange method. The FePMA catalysts were prepared with different ratios of iron and PMA protons (x = 0.17, 0.33, 0.50, 0.67, 0.83, and 1.0). Moreover, the 0.17 FePMA/mSiO2 catalyst was subjected to calcination at different temperatures of 350, 400, and 450 °C. The as-prepared catalysts were characterized through Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction technique(XRD), Transmission electron microscope (TEM), Scanning electron microscope (SEM), and Brunauer-Emmett-Teller technique (BET). The surface acidity of these catalysts was assessed via nonaqueous-potentiometric titration by using n-butylamine. The FT-IR analysis was performed to determine acid sites (Lewis acid and Brønsted acid sites) by chemisorbed pyridine. With increasing iron content, there was a significant reduction in the Brønsted sites and an increase in the Lewis acid sites giving a corresponding decrease in the Brønsted-to-Lewis ratio. Catalytic performance was evaluated through the synthesis of 3,4-dihydropyrimidinone, 7-hydroxy-4-methylcoumarin and hydroquinone diacetate. The results indicated that excessive iron loading diminished catalytic activity and surface acidity due to the reduction in the number of protons from PMA. The highest catalytic performance was achieved using the 0.17 FePMA/mSiO2 catalyst calcined at 350 ℃. Moreover, the as-prepared catalysts were easily eliminated from the mixture of reactions by filtration and demonstrated excellent thermal stability, reusability, and environmental friendliness.
AB - In this study, we synthesized Fe-exchanged phosphomolybdic acid catalysts supported by mesoporous SiO2 (FePMA/mSiO2) using an ion-exchange method. The FePMA catalysts were prepared with different ratios of iron and PMA protons (x = 0.17, 0.33, 0.50, 0.67, 0.83, and 1.0). Moreover, the 0.17 FePMA/mSiO2 catalyst was subjected to calcination at different temperatures of 350, 400, and 450 °C. The as-prepared catalysts were characterized through Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction technique(XRD), Transmission electron microscope (TEM), Scanning electron microscope (SEM), and Brunauer-Emmett-Teller technique (BET). The surface acidity of these catalysts was assessed via nonaqueous-potentiometric titration by using n-butylamine. The FT-IR analysis was performed to determine acid sites (Lewis acid and Brønsted acid sites) by chemisorbed pyridine. With increasing iron content, there was a significant reduction in the Brønsted sites and an increase in the Lewis acid sites giving a corresponding decrease in the Brønsted-to-Lewis ratio. Catalytic performance was evaluated through the synthesis of 3,4-dihydropyrimidinone, 7-hydroxy-4-methylcoumarin and hydroquinone diacetate. The results indicated that excessive iron loading diminished catalytic activity and surface acidity due to the reduction in the number of protons from PMA. The highest catalytic performance was achieved using the 0.17 FePMA/mSiO2 catalyst calcined at 350 ℃. Moreover, the as-prepared catalysts were easily eliminated from the mixture of reactions by filtration and demonstrated excellent thermal stability, reusability, and environmental friendliness.
KW - Coumarin derivatives
KW - Dihydropyrimidinone
KW - Heteropoly acids
KW - Hydroquinone diacetate
KW - Mesoporous Materials
KW - Surface acidity
UR - http://www.scopus.com/inward/record.url?scp=85216986962&partnerID=8YFLogxK
U2 - 10.1016/j.inoche.2025.114045
DO - 10.1016/j.inoche.2025.114045
M3 - Article
AN - SCOPUS:85216986962
SN - 1387-7003
VL - 174
JO - Inorganic Chemistry Communications
JF - Inorganic Chemistry Communications
M1 - 114045
ER -