In the present paper, a novel and benign protocol for microwave enhanced one pot syntheses of 2,3‐dihydro‐1,5 benzodiazepine derivatives from substituted acetophenones, aryl‐aldehydes and o‐phenylene diamine using heterogeneous calcium ferrite/graphene oxide (CF/GO) nanocomposite has been reported. The catalyst was prepared by ultrasonication method and characterized by spectral and analytical techniques. The CF/GO nanocomposite was employed for environmentally benign synthesis of 2,3‐dihydro‐1,5 benzodiazepines. The synthesized benzodiazepine derivatives were screened for their antimicrobial activities against various bacteria and fungi. The present synthetic strategy offered several advantages such as excellent yields in short span of time, simple modus operandi, ease of isolation and purification of products, simple recovery and reusability of the catalyst. A tentative mechanism for synthesis of 2,3‐dihydro‐1,5 benzodiazepine using CF/GO nanocatalyst has also been proposed.