Magnetically retrieval CuFe2O4@MIL‐101(Cr) metal–organic framework was successfully prepared from easily available starting materials and characterized using various spectroscopic and analytical techniques such as powder X‐ray diffraction, scanning electron microscopy, energy dispersive X‐ray, transmission electron microscopy, elemental mapping, Fourier transform infrared spectroscopy, thermogravimetric analysis, X‐ray photoelectron spectroscopy, Brunauer–Emmett–Teller, vibrating sample magnetometer, and inductively coupled plasma optical emission spectroscopy. The catalyst was then used in the synthesis of benzodiazepines containing a triazole moiety in water. The advantages of this protocol include high yields, reusability of the catalyst, and gram‐scale synthesis.