Acetolysis of epichlorohydrin (ECH) with acetic acid yields the product 1-acetoxy-3-chloro-2-propanol, which is used for the manufacture of various polyepoxy materials. The conventional method of producing 1-acetoxy-3-chloro-2propanol uses sulfuric acid, p-toluenesulfonic acid, or BF3Et2O as a catalyst. These processes suffer from problems associated with the use of highly corrosive liquid acids. It is thus clear that there is tremendous scope for developing a new catalytic process for the acetolysis of ECH. In the present study, acetolysis of ECH with acetic acid was studied over nanocrystalline ZSM-5 catalysts and was found to be very active for the selective formation of 1-acetoxy-3-chloro-2-propanol. The catalyst was fully characterized. The best parameters for the acetolysis of ECH were established.