反应详情

温度

70 °C

A mixture of 5-nitro-3-(3-methylpyrazol-1-yl)-1,2-benzisothiazole (3.12 g, 12.0 mmol), sodium bicarbonate (2.00 g, 23.8 mmol), acetonitrile and water is stirred one hour at 70° C. and treated with sodium hydrosulfite (8.70 g, 50.0 mmol) in portions. The resultant mixture is stirred overnight at reflux, cooled to room temperature and diluted with ethyl acetate. The organic layer is dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue is washed with a mixture of methylene chloride and ethyl acetate. The organic layer is decanted to afford the title compound as a viscous brown oil which is identified by NMR spectral analysis.

1. temperatureat reflux
2. temperaturecooled to room temperature
3. dry with materialThe organic layer is dried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. washThe residue is washed with a mixture of methylene chloride and ethyl acetate
6. customThe organic layer is decanted