反应详情

温度

0 °C

3-Bromo-6-chloro-imidazo[1,2-b]pyridazine (1.327 g, 5.71 mmol) was dissolved THF (40 mL) and under nitrogen conditions, it was cooled down to 0° C. and ethylmagnesium bromide solution (1 M, 6.85 mL) was added. The RM was stirred at rt for 30 min then a solution of 7-fluoro-quinoline-6-carbaldehyde (Intermediate B), (1.0 g, 5.71 mmol) in THF (20 mL) was added by 0° C. The RM was stirred at rt for 2 h. The solvent was partially removed by evaporation and water (40 mL) was added to the residual mash. After 1 h stirring, the crystallized product was filtered and dried overnight under vacuum to afford the title compound as a powder (tR 3.70 min (conditions 3), MH+=329, 1H-NMR in DMSO-d6: 8.90 (dd, 1H); 8.46 (d, 1H); 8.29-8.23 (m, 2H); 7.72 (d, 1H); 7.54-7.49 (m, 2H); 7.40 (d, 1H); 6.56-6.49 (m, 2H)).

1. stirringThe RM was stirred at rt for 2 h
2. customThe solvent was partially removed by evaporation and water (40 mL)
3. additionwas added to the residual mash
4. stirringAfter 1 h stirring
5. filtrationthe crystallized product was filtered
6. customdried overnight under vacuum