反应详情

温度

170 °C

6-Chloro-3-[(S)-1-(4,6-difluoro-1-methyl-1H-indazol-5-yl)-ethyl]-imidazo[1,2-b]pyridazine (Intermediate Q, 50 mg, 0.144 mmol), KF, 42.6 mg, 0.719 mmol) and piperazin-2-one (44.5 mg, 0.431 mmol) were suspended in NMP (0.3 mL). The RM was stirred at 170° C. for 3 h. The mixture was diluted with EtOAc and washed with NaHCO3 10% (2×) and water (4×). The combined organic layers were dried over Na2SO4, filtered and concentrated. The residue was purified by flash chromatography and then crystallized in EtOAc/Pentane to afford the title compound as a light brown solid (tR 3.63 min (conditions 5), (tR 10.82 min (conditions 2), MH+=412.2, 1H-NMR in DMSO-d6: 8.07 (s, 1H); 8.03 (s, 1H); 7.79 (d, 1H); 7.52 (s, 1H); 7.36 (d, 1H); 7.02 (d, 1H); 4.85 (m, 1H); 3.95 (d, 1H); 3.95 (s, 3H); 3.73 (d, 1H); 3.54 (m, 2H); 3.17 (m, 2H); 1.79 (d, 3H)).

1. washwashed with NaHCO3 10% (2×) and water (4×)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by flash chromatography
6. customcrystallized in EtOAc/Pentane