Novel, reusable, and efficient (Cd, Zn) S nanocatalysts were prepared by simple and economical chemical bath deposition using a greener approach. The as-synthesized catalysts were characterized by XRD, SEM, TEM, and FT-IR spectroscopy. The catalytic activity of as-prepared nanocatalysts were examined for the synthesis of 1,5-benzocliazepines and its derivatives under solvent-free conditions without using any toxic materials. It has been observed that CdS nanocatalyst shows superior catalytic activity and is recyclable and reusable for ten runs without any significant loss.