Graphite-like layered material of composition BC₂N was prepared by the CVD reaction of acetonitrile with boron trichloride at 2070 K. Sodium was intercalated into the BC₂N film and powder by two methods: a vapor phase reaction and an electrochemical method. The first stage compounds were prepared by the vapor phase reaction using the BC₂N film and powder. A mixture of the first and the second stage compounds was prepared from the BC₂N powder, while the first stage compound was prepared from the BC₂N film by the electrochemical method. The d-spacing of the intercalated layers was 0.43 nm, calculated from the sharp (001) and (002) diffraction lines observed on the X-ray diffraction patterns of the first stage compounds prepared from the BC₂N films by the two methods.