反应详情

温度

110 °C

To a solution of 1-(6-chloroimidazo[1,2-b]pyridazin-3-yl)-1-(7-fluoroquinolin-6-yl)ethanol (420 mg, 1.10 mmol) in acetic acid (20 mL) was added phosphinic acid (50% aqueous solution, 0.60 ml, 5.51 mmol) and iodine (700 mg, 2.76 mmol). The resulting solution was heated at 110° C. overnight and the solvent was removed. The residue was diluted with water and pH was adjusted to 8-10 with 6N NaOH solution. The mixture was then extracted by CH2Cl2, washed with brine, dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by column chromatography (3% to 10% MeOH in CH2Cl2) to afford 260 mg (yield: 72%) title compound. LCMS (method B): [MH]+=327, tR=2.52 min.

1. customthe solvent was removed
2. additionThe residue was diluted with water and pH
3. extractionThe mixture was then extracted by CH2Cl2
4. washwashed with brine
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by column chromatography (3% to 10% MeOH in CH2Cl2)