反应详情

温度

65 °C

A solution of 3-chloro-6-(3-fluoro-phenyl)-[1,2,4]triazine (2.09 g, 10.0 mmol) in 13.6 ml of dry pyridine was cooled to 0° C. with ice bath and 1.7 ml of hydrazine hydrate was added. The mixture was then heated to 65° C. and maintained this temperature for ca. 0.5 hour. After cooling down to room temperature, the mixture was poured into ice-water. The resulting solid was recovered by filtration and washed well with water, dried and scratched with hexane to give title compound (1.85 g, 90.2%) as a yellow crystalline solid: 1H NMR (DMSO-d6): δ 8.97 (b, 1H), 8.90 (s, 1H), 7.89-7.82 (m, 2H), 7.59-7.51 (m, 1H), 7.30-˜7.24 (m, 1H), 5.47 (b, 2H); MS (m/z) 206 [M+H+]+.

1. temperaturemaintained this temperature for ca. 0.5 hour
2. temperatureAfter cooling down to room temperature
3. filtrationThe resulting solid was recovered by filtration
4. washwashed well with water
5. customdried