Highly efficient CuI nanoparticles catalyzed one-pot synthesis of some benzo [b][1,5]diazepine derivatives via multicomponent condensation of aromatic diamines, Meldrum's acid and isocyanides. The present approach creates a variety of benzo [b][1,5]diazepines as pharmaceutical and biologically active heterocyclic compounds in excellent yields and short reaction times. The salient features of the copper iodide nanoparticles are: easy preparation, cost-effective, high stability, low loading and reusability of the catalyst. The prepared copper iodide nanoparticles were fully characterized by XRD, EDX, FT-IR, SEM and TEM analysis.