3, 5-Dimethylisoxazole (1) was alkylated with sodium amide in liquid ammonia to give 3- methyl-5-alkylisoxazoles. By di-and tri-alkylation reactions using excess sodium amide, isoxazoles having secondary and tertiary alkyl groups at 5-position could be obtained. The hydrogenolysis and hydrolysis of these isoxazoles were also studied.