反应详情

温度

75 °C

A 100 mL round bottomed flask equipped with a magnetic stir bar is charged {(3S)-3-[(benzylamino)methyl]-6-nitro-2,3-dihydro-1,4-benzodioxin-5-yl}acetonitrile (5.00 g, 14.5 mmol) and 95% ethanol (7.5 mL). To the stirred solution is added 95% sulfuric acid (5.0 mL, 89.0 mmol). The flask is immersed in an oil bath and heated to 75° C. for 4 days. The solution is cooled to room temperature and absolute ethanol (42.5 mL) is added. The reaction mixture is adjusted to pH 10 by the addition of 28% ammonium hydroxide (˜12 mL), and the resulting slurry is stirred for 3 h. The precipitate is removed by vacuum filtration and the volatiles are evaporated giving crude title compound (6.02 g, 106%) as a red syrup. LCMS (Basic Method): 2.33 min, 387 (M+H)+.

1. customA 100 mL round bottomed flask equipped with a magnetic stir bar
2. customThe flask is immersed in an oil bath
3. temperatureThe solution is cooled to room temperature
4. customThe precipitate is removed by vacuum filtration
5. customthe volatiles are evaporated