The synthesis of 6-methoxy-2-naphthaldehyde (Ⅰ) was explored. The treatment of 2-acetyl-6-methoxynaphthalene (Ⅱ) with sodium hypochlorite resulted in the formation of 6-methoxy-2-naphthoic acid (Ⅲ). Esterifying of compound Ⅲin the presence of CH3OH/H2SO4 afforded 6-methoxy-2-naphthoate (Ⅳ), followed by Red-Al reduction of the ester group, led to 6-methoxy-2-naphthyl methanol (Ⅴ), a selective oxidation was then performed with MnO2 to provide the target compound 6-methoxy-2-naphthaldehyde (Ⅰ) in an overall yield of 73.2%. The structure of Ⅰ was characterized by MS and 1H NMR.