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We report here the preparation of 2-hydroxy-5-iodo-N’-(1-arylethylidene)benzohydrazide compounds in good to excellent yields (83–98%) within a short reaction time (10–15 min), through a clean and efficient procedure. Seventeen new compounds were synthesized and fully characterized by FT-IR, NMR, and HRMS. The deep eutectic solvent can be recovered easily by phase extraction and can be reused up to several times without any significant loss of catalytic activity. Additionally, the method has a wide substrate scope and provides an accessible route for the large-scale direct synthesis of 2-hydroxy-5-iodo-N’-(1-arylethylidene)benzohydrazides.