反应详情

To a stirred solution of 3-methylthio-4H-1,2,4-triazole (1.00 g; Oakwood Products, Inc., West Columbia, S.C.) in THF (20 mL) and water (20 mL) was added potassium peroxomonosulfate (Oxone®, DuPont Specialty Chemicals, Deepwater, N.J., USA) (10.7 g). After stirring at room temperature for a day, the reaction mixture was filtered and the filtercake was washed with THF. The filtrate was partitioned between water and ethyl acetate, the bilayer was separated and the aqueous portion was extracted twice with ethyl acetate. The combined organic extracts were dried over MgSO4, filtered, and the filtrate concentrated under reduced pressure. The resulting residue was purified by flash chromatography (SiO2, ethyl acetate/methanol, 0-10%) to afford 0.496 g of (I-5a) as a white solid. m/z 148.1 (M+H)+.

1. filtrationthe reaction mixture was filtered
2. washthe filtercake was washed with THF
3. customThe filtrate was partitioned between water and ethyl acetate
4. customthe bilayer was separated
5. extractionthe aqueous portion was extracted twice with ethyl acetate
6. dry with materialThe combined organic extracts were dried over MgSO4
7. filtrationfiltered
8. concentrationthe filtrate concentrated under reduced pressure
9. customThe resulting residue was purified by flash chromatography (SiO2, ethyl acetate/methanol, 0-10%)
10. customto afford 0.496 g of (I-5a) as a white solid