反应详情

温度

75 °C

To a solution of (E)-3-(4-((E)-2-phenyl-1-(1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-yl)but-1-en-1-yl)phenyl)acrylonitrile (380 mg, 0.83 mmol) and hydroxylamine hydrochloride (265 mg, 3.8 mmol) in DMSO (8 mL) was added triethylamine (0.5 mL, 3.8 mmol), and the mixture was heated at 75° C. for 24 h. After cooling, water was added, and the solution was extracted with EtOAc (3×). The combined organics were washed with brine (2×), dried (MgSO4) and concentrated. Purification by silica gel chromatography (0 to 65% EtOAc/hexanes) provided 116 mg of the title compound as a yellow foam. LCMS: 409 [(M-THP+H)+H]+.

1. temperatureAfter cooling
2. extractionthe solution was extracted with EtOAc (3×)
3. washThe combined organics were washed with brine (2×)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customPurification by silica gel chromatography (0 to 65% EtOAc/hexanes)