反应详情

温度

65 °C

A solution of 6-fluoro-3-methyl-5-nitro-1,2-benzisothiazole (0.740 g, 3.50 mmol), 5% acetic acid (25.0 mL) and ethyl acetate is heated to 65° C., treated with iron powder (0.980 g, 17.5 mmol), stirred at 65° C. for one hour, cooled to room temperature, and filtered to remove solids. The organic phase is separated, washed sequentially with water, saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as an orange solid (0.610 g) which is identified by NMR spectral analyses.

1. temperaturecooled to room temperature
2. filtrationfiltered
3. customto remove solids
4. customThe organic phase is separated
5. washwashed sequentially with water, saturated sodium hydrogen carbonate solution and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo