反应详情

温度

120 °C

A mixture of 1-(6-chloroimidazo[1,2-b]pyridazin-3-yl)-1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethanol (1.1 g, 3.18 mmol), diiodine (2.019 g, 7.95 mmol), and phosphinic acid (0.840 g, 12.73 mmol) in HOAc (10 ml) was heated to 120° C. for 5 h. After cooling to rt, the reaction mixture was concentrated in vacuo. The residue was taken with water and adjusted its pH tp 8 with aqueous NaOH. The mixture was extracted with DCM, dried over Na2SO4 and concentrated to give a residue, which was purified with silica gel column chromatography (MeOH:EA) to give 6-chloro-3-(1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethyl)imidazo[1,2-b]pyridazine (900 mg 60%). LCMS (method B): [MH]+=330, tR=2.59 min.

1. temperatureAfter cooling to rt
2. concentrationthe reaction mixture was concentrated in vacuo
3. extractionThe mixture was extracted with DCM
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customto give a residue, which
7. customwas purified with silica gel column chromatography (MeOH:EA)