The mechanochemical route is a facile and fast way and has received much attention for developing versatile advanced functional materials. Herein, we reported a mechanochemical synthesis for incorporating divalent manganese ions (Mn II ) into a two-dimensional (2D) hybrid perovskite (C 4 H 9 NH 3 ) 2 PbCl 4 . The mild external stimuli originating from the grinding at room temperature enabled the formation of Mn II -doped 2D hybrid perovskites, and rapidly changed the luminescence characteristics. The photoluminescence analyses show that the violet and orange emissions are attributed to (C 4 H 9 NH 3 ) 2 Pb 1-x Mn x Cl 4 band-edge emission and the T 1 → 6 A 1 transition of Mn 2+ resulting from an efficient energy transfer process, respectively. Site preference and distribution of the doped Mn 2+ cations on the locations of Pb 2+ were analyzed. The formation energy calculated by the density functional theory (DFT) indicates that the Mn 2+ ions can rapidly enter the crystal lattice due to the unique 2D crystal structure of the hybrid perovskite. Such a case of mechanochemical synthesis for the 2D hybrid perovskite motivates many novel emerging materials and the related applications.