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This study describes an efficient and solvent-free method for the regioselective production of L-lysine ammonium epsilon-carbamate by ball-milling L-lysine under an atmosphere of CO<sub>2</sub>. The regioselective formation of L-lysine ammonium epsilon-carbamate by this mechanochemical approach was confirmed by a complete analytical study, including <sup>1</sup>H-<sup>13</sup>C and <sup>1</sup>H-<sup>15</sup>N CP MAS NMR measurements as well as liquid NMR analysis, powder X-ray diffraction,doi:10.26434/chemrxiv.11336087 fatcat:vv7pkc4e2nh3tp3fq32bvf44ei