反应详情

温度

38 °C

To a stirred suspension of (6-chloro-imidazo[1,2-b]pyridazin-3-yl)-(6-fluoro-1-methyl-1H-indazol-5-yl)-methanone ((ii), 25.45 g, 74 mmol) and THF (4 L) was added methyl magnesium bromide (3 M, 43 mL) at 38° C. during 15 min. The mixture was stirred at 38° C. for 20 min. The RM was cooled to RT, quenched with 1M NaHCO3 and extracted with EtOAc (3×). The organic layers were washed with brine, dried over Na2SO4, filtered and concentrated. The title compound was obtained after crystallization in DCM-TBME (1:2) as a beige solid (tR 3.30 min (conditions 1); MH+=346).

1. temperatureThe RM was cooled to RT
2. customquenched with 1M NaHCO3
3. extractionextracted with EtOAc (3×)
4. washThe organic layers were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated