Hydrotalcite, also known as aluminum-magnesium layered double hydroxide (LDH) or anionic clay, is a synthetic compound that was broadly investigated in the past decade due to its many potential applications. In this work, we present an environmentally benign process for the transesterification (methanolysis) of neem oil to fatty acid methyl esters (FAME) using Zn-Mg-Al hydrotalcites as solid base catalysts in a heterogeneous manner. The catalysts were characterized by XRD, FT-IR, TPD-CO2, and the BET surface area analysis. It is well-known that the catalytic performance of hydrotalcite is dramatically increased through the incorporation of Zn into the surface of Mg-Al hydrotalcite material. The optimized parameters, 10 : 1 methanol/oil molar ratio with 7.5 g catalysts reacted under stirring speed 450 rpm at 65°C for 4 h reaction, gave a maximum ester conversion of 90.5% for the sample with Zn-Mg-Al ratio of 3 : 3 : 1.