A distinctive two-dimensional (2D) melting transition occurring at nearly 100 degrees Celsius (degrees C) has been observed in Langmuir-Blodgett films by in situ atomic force microscopy (AFM). A 2D orthorhombic crystal phase melted to a 2D smectic phase at about 91 degrees C. The smectic phase was characterized by 1D molecular periodicity with short-range correlations (about 40 angstroms). At 95 degrees C, the smectic order melted! to form a hexatic phase. infrared spectroscopy measurements were consistent with the AFM observations. These observations support the dislocation-mediated melting scenario for an anisotropic 2D crystal predicted by Ostlund and Halperin. A longer wavelength height modulation was also observed in the smectic and hexatic phases.