10557-85-4

300-87-8

10557-85-4

General procedure for the synthesis of 3,5-dimethyl-4-iodoisoxazole from 3,5-dimethylisoxazole: 1. Preparation of Intermediate 1 (4-iodo-3,5-dimethylisoxazole): Nitric acid (13 mL) was slowly added dropwise (note the exothermic reaction) to a mixture containing 3,5-dimethylisoxazole (31.3 g, 320 mmol) and iodine (37.3 g, 150 mmol) at room temperature. After dropwise addition, the reaction mixture was continued to be stirred for 1 hour. 2. Post-treatment: The reaction mixture was quenched with a mixture of ice and water followed by extraction with dichloromethane (DCM). The organic phase was separated, washed with sodium thiosulfate (Na2S2O3) solution and dried over anhydrous sodium sulfate (Na2SO4). Finally, the organic phase was concentrated under reduced pressure to afford the target product 3,5-dimethyl-4-iodoisoxazole as a yellow solid (60 g, 83% yield). [APCI MS] m/z: 224 [M+H]+, retention time (Rt) 2.17 min.