A new layered-structure compound, BC 2N, has been synthesized by a vapor-phase reaction of CH 3CN and BCl 3. The electrochemical behavior of BC 2N as a negative electrode matrix of a rechargeable lithium battery was investigated in organic electrolyte solutions containing lithium salts. Cyclic voltammetry and X-ray diffraction analysis showed that the electrochemical intercalation/deintercalation of lithium in the BC 2N electrode is applicable to the negative electrode reaction for a rechargeable battery with a high-energy density. A thermal treatment after the BC 2N synthesis drastically changed the crystal structure of BC 2N and the electrochemical charge/discharge characteristics in propylene carbonate-based electrolytes. A 100% coulombic efficiency was obtained for the BC 2N electrode treated at 1500 °C.