反应详情

温度

50 °C

A suspension of 1,1-dimethylethyl 7-cyano-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (may be prepared as described in WO2002040471) (5 g, 18.36 mmol), hydroxylamine hydrochloride (2.55 g, 36.7 mmol) and sodium bicarbonate (7.71 g, 92 mmol) in ethanol (250 ml) was heated at 50° C. overnight. Further hydroxylamine hydrochloride (0.638 g, 9.18 mmol) was added to the reaction mixture and heating at 50° C. continued for 5 h. The reaction mixture was allowed to cool and the solid filtered off, the solution was concentrated in vacuo to yield the title compound as a white solid (5.77 g, 17.01 mmol, 93% yield). δH (d6DMSO, 400 MHz): 9.56 (1H, s), 7.52-7.37 (2H, m), 7.14 (1H, d), 5.77 (2H, br s), 3.50-3.32 (4H, m), 2.91-2.80 (4H, m), 1.41 (9H, s). MS (ES): C16H23N3O3 requires 305; found 306 [M+H]+.

1. temperatureheating at 50° C.
2. temperatureto cool
3. filtrationthe solid filtered off
4. concentrationthe solution was concentrated in vacuo