反应详情

To a CHCl3 (20 mL) solution of N-(6-chloroimidazo[1,2-b]pyridazin-2-yl)acetamide (320.4 mg, 1521 μmol) was added n-iodosuccinimide (167.4 μl, 1673 μmol) as a solid in a single portion. The solution was maintained at rt for 20 min, then poured into water. The resulting mixture was extracted with CH2Cl2 (1×50 mL). The layers were separated and the organic layer was washed with saturated aqueous Na2S2O3 (1×20 mL) and brine (1×10 mL). The organic layer was dried (Na2SO4) and concentrated for purification by MPLC (CombiFlash® Companion®, Teledyne Isco, Lincoln, Nebr.). The residue was taken up in minimal CH2Cl2/MeOH and absorbed onto a 25 g silica loading cartridge and passed through a Redi-Sep® pre-packed silica gel column (80 g) (Teledyne Isco, Lincoln, Nebr.) using a gradient of 1% MeOH in CH2Cl2 to 10% MeOH in CH2Cl2 to afford N-(6-chloro-3-iodoimidazo[1,2-b]pyridazin-2-yl)acetamide (427.0 mg, 83.41% yield) as a grey solid. LCMS (ESI positive ionization) m/z: 337.2 (M+1).

1. extractionThe resulting mixture was extracted with CH2Cl2 (1×50 mL)
2. customThe layers were separated
3. washthe organic layer was washed with saturated aqueous Na2S2O3 (1×20 mL) and brine (1×10 mL)
4. dry with materialThe organic layer was dried (Na2SO4)
5. concentrationconcentrated for purification by MPLC (CombiFlash® Companion®, Teledyne Isco, Lincoln, Nebr.)
6. customabsorbed onto a 25 g silica loading cartridge