5-Hydroxy-1,4-naphthoquinone and its derivatives were evaluated for insecticidal effect against Sitophilus oryzae and S. zaemais adults. This study was examined using fumigant method. Mortality was determined after 72 h of treatment. 5-Hydroxy-1,4-naphthoquinone showed strong (+++) activity at 5 mg and the 1,4-naphthoquinone showed strong (+++) and moderate (++) activity at 5 mg, against S. oryzae and S. zaemais, respectively. However, 5-hydroxy-2-methyl-1,4-naphthoquinone, 2-methyl-1,4-naphthoquinone, 2-hydroxy-1,4-naphthoquinone, and 2-methoxy-1,4-naphthoquinone had non-activity (-) at 5 mg. Based on the LD50 values, the compound most highly effect to S. oryzae was 1,4-naphthoquinone (0.012 mg/cm2), followed by 5-hydroxy-1,4-naphthoquinone (0.013 mg/cm2). However, against S. zeamais, 5-hydroxy-1,4-naphthoquinone (0.044 mg/cm2) was the most toxic compound, followed by 1,4-naphthoquinone (0.155 mg/cm2). These results suggest that the introduction of various functional group (hydroxy, methyl and methoxy) into the 1,4-naphthoquinone skeleton contributes to insecticidal activity. Accordingly, 5-hydroxy-1,4-naphthoquinone and 1,4-naphthoquinone could be used highly effective rice weevil control agents.