反应 #77285

反应方程式

1-methyl-3-[3-[4-[(methylthio)methyl]-1,3-dioxolan-2-yl]-1,2-benzisothiazol-5-yl]-6-(trifluoromethyl)uracil

m-chloroperbenzoic acid

→

title compound

收率 70.0%

1-Methyl-3-[3-[4-[(methylsulfinyl)methyl]-1,3-dioxolan-2-yl]-1,2-benzisothiazol-5-yl]-6-(trifluoromethyl)uracil

收率 70.0%

溶剂

methylene chloride

反应条件

后处理

1. 1
   浓缩concentrated in vacuo
2. 2
   洗涤washed twice with 5% aqueous sodium carbonate and once with brine
3. 3
   干燥The organic layer is dried over anhydrous magnesium sulfate
4. 4
   浓缩concentrated in vacuo to a white solid, which
5. 5
   其他is chromatographed on silica gel with ethanol-ethyl acetate

实验过程

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.

来源