反应详情

To a mixture of 3-[3-[5-(bromomethyl)-5-hydroxy-m-dioxan-2-yl]-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)uracil (0.580 g, 1.11 mmol) and tetrahydrofuran at 5° C. is added sodium hydride (60% dispersion in mineral oil, 0.0400 g, 1.11 mmol). The resultant mixture is stirred overnight at ambient temperature and treated with additional sodium hydride (0.0400 g, 1.11 mmol). The mixture is poured into saturated ammonium chloride and extracted twice with diethyl ether. The combined organic extracts are washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue is chromatographed on silica gel with diethyl ether-methylene chloride to afford the title compound (0.0800 g, 16.3%, mp 203-206° C.) which is identified by NMR spectral analysis.

1. extractionextracted twice with diethyl ether
2. washThe combined organic extracts are washed with water and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue is chromatographed on silica gel with diethyl ether-methylene chloride