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This manuscript presents the ultrasound-assisted synthesis of 4H-furo[3,4-b]pyran derivatives using a novel catalyst composed of an Fe3O4-supported Schiff base-Ni(II) complex. The incorporation of ultrasound technology significantly enhances the efficiency and yields of the reaction, highlighting a green chemistry approach to synthesizing these biologically significant compounds. The synthesized derivatives were characterized using various spectroscopic techniques to confirm their structural integrity and purity. Furthermore, the catalytic performance of the Fe3O4-supported complex was evaluated, demonstrating its effectiveness in promoting the reaction under mild conditions. This study not only highlights the potential of ultrasound-assisted methodologies in organic synthesis and emphasizes the usefulness of metal–organic frameworks in catalysis, paving the way for further exploration of sustainable synthetic strategies for complex organic molecules. [ABSTRACT FROM AUTHOR]