反应详情

A solution of 4-(1H-indazol-6-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (9.70 g, 3.24 mmol) in DMF (32 mL) at room temperature was treated with iodine (1.23 g, 4.86 mmol) and KOH (grounded, 454 mg, 8.1 mmol). The resulting mixture was stirred at room temperature for 40 min, then treated with saturated Na2S2O3 aqueous solution. The resulting mixture was then extracted with EtOAc (3×). The combined extracts were washed with brine and dried over Na2SO4. The resulting mixture was filtered and concentration under reduced pressure. The resulting residue was purified by flash chromatography on silica-gel (gradient eluant 10% to 40% EtOAc in heptane) to yield the title compound as white solid.

1. extractionThe resulting mixture was then extracted with EtOAc (3×)
2. washThe combined extracts were washed with brine
3. dry with materialdried over Na2SO4
4. filtrationThe resulting mixture was filtered
5. concentrationconcentration under reduced pressure
6. customThe resulting residue was purified by flash chromatography on silica-gel (gradient eluant 10% to 40% EtOAc in heptane)