反应详情

A solution of (6-chloroimidazo[1,2-b]pyridazin-3-yl)(1-methyl-1H-indazol-5-yl)methanol (156.8 mg, 0.50 mmol), I2 (381 mg, 1.50 mmol) and H3PO2 (0.273 mL, 2.50 mmol) in 4 mL AcOH was heated at 110° C. for 7 hours. The solvent was removed under reduced pressure. The residue was diluted with water and extracted with DCM twice. The organic layers were combined, dried over Na2SO4 and concentrated. The crude product was purified by flash chromatography (DCM:MeOH=20:1) to give the title compound which contains some iodine and used in the next step without further purification (180.0 mg, 44%, 36% pure). LCMS (method A): [MH]+=298, tR=5.37 min

1. customThe solvent was removed under reduced pressure
2. additionThe residue was diluted with water
3. extractionextracted with DCM twice
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe crude product was purified by flash chromatography (DCM:MeOH=20:1)