反应详情

To a solution of 5-chloro-4-iodo-3-(pentan-3-ylamino)picolinonitrile (55 mg, 0.16 mmol) in DMSO (1 mL) was added solid potassium carbonate (210 mg, 0.64 mmol). The mixture was cooled in an ice water bath (0° C.) and aqueous hydrogen peroxide (30%, 0.5 mL) was added. The reaction was allowed to warm to room temperature and monitored by LCMS. After the reaction was complete, the reaction mixture was diluted with EtOAc, and the organic layer was washed repeatedly with water. The organic layer was then dried over sodium sulfate, filtered and concentrated in vacuo. The residue was filtered through a silica gel plug to provide the title compound as a white solid (50 mg, 83%). The compound was characterized by LCMS (m/z=368.1 [M+H]+) and 1H NMR.

1. additionwas added
2. washthe organic layer was washed repeatedly with water
3. dry with materialThe organic layer was then dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. filtrationThe residue was filtered through a silica gel plug