反应详情

温度

110 °C

Iodine (3.09 g, 12.17 mmol) and H3PO2 (1.673 mL of a 50% aqueous solution, 30.4 mmol) are added to a solution of (rac)-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-(7-fluoro-quinolin-6-yl)methanol (Stage 174.3, 2 g, 6.08 mmol) in acetic acid (20 mL). The RM was heated under stirring at 110° C. for 18 h. The RM was then evaporated and taken into DCM and washed with NaHCO3 sol., and extracted with DCM/NaHCO3 sol. The combined organic layer were dried and concentrated. The residue was stirred in acetone and filtered. After 3 h drying under vacuum, it gave the title compound (tR 4.41 min (conditions 3), MH+=313).

1. temperatureThe RM was heated
2. customThe RM was then evaporated
3. washwashed with NaHCO3 sol.
4. extractionextracted with DCM/NaHCO3 sol. The combined organic layer
5. customwere dried
6. concentrationconcentrated
7. stirringThe residue was stirred in acetone
8. filtrationfiltered
9. customAfter 3 h drying under vacuum, it