反应详情

温度

160 °C

To a solution of (4-bromo-2-cyano-phenyl)-carbamic acid ethyl ester (40.4 g, 150 mmol) in NMP (170 mL) was added formylhydrazine (10.0 g, 150 mmol). The resulting mixture was stirred for 1.5 h at 160° C. under a gentle nitrogen sweep. It was cooled to below 100° C. and water (340 mL) was added slowly. The resulting slurry was cooled to 25° C. and stirred for 15 min. The solid was collected by filtration and washed with water and 2-propanol. Drying in vacuo afforded the title compound (32.4 g, 81%) as a light yellow solid. MS: m/e 264.9/267.0 [M+H+].

1. temperatureIt was cooled to below 100° C.
2. temperatureThe resulting slurry was cooled to 25° C.
3. stirringstirred for 15 min
4. filtrationThe solid was collected by filtration
5. washwashed with water and 2-propanol
6. customDrying in vacuo