反应详情

温度

80 °C

To a mixture of 2-(2,4-difluorophenyl)-3-(2-methanesulfonylpyrimidin-4-yl)-8-methyl-imidazo[1,2-a]pyrazine (1.4 g, 3.5 mmol) in ACN (30 mL) was added 3-amino-2,2-dimethyl-propan-1-ol (Lancaster, 0.79 g, 7.7 mmol). The mixture was heated to about 80° C. After about 16 h, the mixture was treated with additional 3-amino-2,2-dimethyl-propan-1-ol (Lancaster, 0.20 g, 1.9 mmol) and heated at about 80° C. for about another 4 h. The mixture was filtered through a pad of silica gel and eluted with EtOAc. The solution was evaporated, triturated with ether, and then filtered. The solid was dissolved in hot methanol (˜10 mL). The solution was cooled and the solvent evaporated. The resulting solid was dried at 100° C. under vacuum to yield the title compound as a white solid (0.88 g, 59%): LC/MS (Table 1, Method g) Rt=2.38 min; MS m/z: 425.2 (M+H)+, mp 173.8-174.5° C.

1. temperatureheated at about 80° C. for about another 4 h
2. filtrationThe mixture was filtered through a pad of silica gel
3. washeluted with EtOAc
4. customThe solution was evaporated
5. customtriturated with ether
6. filtrationfiltered
7. dissolutionThe solid was dissolved in hot methanol (˜10 mL)
8. temperatureThe solution was cooled
9. customthe solvent evaporated
10. customThe resulting solid was dried at 100° C. under vacuum