反应详情

To a mixture of 2,5-dichloropyrazine (CombiPhos, 2.00 g, 13.42 mmol), ammonium hydroxide (5.05 mL, 38.9 mmol), and water (10.0 mL) was added hydrazine hydrate (1.57 mL, 32.2 mmol). The mixture was heated at reflux for about 17 h, cooled in an ice bath for about 15 min, filtered, washed with ice cold water (3×25 mL), and dried in a vacuum oven at about 70° C. to give the title compound (1.60 g, 78%): LC/MS (Table 1, Method h) Rt=1.07 min; MS m/z: 145.0 (M+H)+.

1. temperatureThe mixture was heated
2. temperatureat reflux for about 17 h
3. temperaturecooled in an ice bath for about 15 min
4. filtrationfiltered
5. washwashed with ice cold water (3×25 mL)
6. customdried in a vacuum oven at about 70° C.