反应详情

A mixture of 1-methyl-3-[3-[4-[(methylthio)methyl]-1,3-dioxolan-2-yl]-1,2-benzisothiazol-5-yl]-6-(trifluoromethyl)uracil (0.970 g, 21.1 mmol), m-chloroperbenzoic acid (72%, 0.500 g, 21.1 mmol) and methylene chloride is stirred one hour at room temperature and concentrated in vacuo. The residue is taken up in ethyl acetate and washed twice with 5% aqueous sodium carbonate and once with brine. The organic layer is dried over anhydrous magnesium sulfate and concentrated in vacuo to a white solid, which is chromatographed on silica gel with ethanol-ethyl acetate to afford the title compound as a white solid (0.700 g, 70.0%, mp 72-75° C.) which is identified by IR and NMR spectral analysis.

1. concentrationconcentrated in vacuo
2. washwashed twice with 5% aqueous sodium carbonate and once with brine
3. dry with materialThe organic layer is dried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo to a white solid, which
5. customis chromatographed on silica gel with ethanol-ethyl acetate