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Amylopectin (Ap) was grafted with three different methacrylate by atom transfer radical polymerization (ATRP) to create controllable hydrophobic chain on amylopectin. The macro initiator Amylopectin-Ethyl α-bromoisobutyrate (Ap-EBiB) was prepared by esterification of hydroxyl groups on amylopectin with Ethyl α-Bromoisobutyrate (EBiB). In this research, amylopectin was grafted with methyl methacrylate (MMA), butyl methacrylate (BMA) and hexyl methacrylate (HMA) and the grafting conditions were optimized. Influence of grafting conditions on % monomer conversion, and % grafting efficiency were studied. Grafted samples were analyzed for their thermal behavior using thermo gravimetric analysis (TGA) and differential scanning calorimeter (DSC) and grafting was confirmed using nuclear magnetic resonance (NMR), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). It was found that increasing length of alkyl chains increased grafting efficiency but improved the thermal behavior with better properties. The result of this study indicated that the Amylopectin-g-PHMA have % grafting higher than others. [ABSTRACT FROM AUTHOR]