反应详情

温度

80 °C

To a mixture of 2-(4-fluorophenyl)-3-(2-methanesulfonylpyrimidin-4-yl)-8-methylimidazo[1,2-a]pyrazine (1.50 g, 391 mmol) in ACN (30 mL) was added 3-amino-2,2-dimethyl-1-propanol (Lancaster, 2.0 g, 20 mmol). The reaction mixture was heated to about 80° C. After about 1.5 h, the reaction was cooled to ambient temperature and concentrated under reduced pressure. The resulting crude material was purified by silica gel chromatography with DCM/MeOH/NH4OH (step-wise gradient, 990:9:1 then 980:18:2) to give an oil after concentration. The oil was dissolved in a minimum amount of DCM and heptane was added until a white precipitate formed. The suspension was concentrated under reduced pressure. The resulting solid was triturated with heptane and filtered to give the title compound (1.36 g, 86%): LC/MS (Table 1, Method g) Rt=2.41 min; MS m/z: 407.2 (M+H)+.

1. temperaturethe reaction was cooled to ambient temperature
2. concentrationconcentrated under reduced pressure
3. customThe resulting crude material was purified by silica gel chromatography with DCM/MeOH/NH4OH (step-wise gradient, 990:9:1
4. custom980:18:2) to give an oil
5. concentrationafter concentration
6. dissolutionThe oil was dissolved in a minimum amount of DCM and heptane
7. additionwas added until a white precipitate
8. customformed
9. concentrationThe suspension was concentrated under reduced pressure
10. customThe resulting solid was triturated with heptane
11. filtrationfiltered