反应详情

温度

70 °C

step 5—A mixture of 86 (0.050 g, 0.11 mmol), 48% HBr (0.050 mL) and AcOH (2 mL) in a sealed tube was heated overnight at 70° C. The reaction mixture was cooled to RT, carefully poured into a cold saturated aqueous NaHCO3 and then extracted with EtOAc. The organic layer was washed with brine, dried (MgSO4) and concentrated. The crude residue was purified by SiO2 chromatography and eluted with 10% MeOH/DCM to afford 32 mg (66%) of N-(4-{2-[2-amino-5-tert-butyl-3-(2-oxo-1,2-dihydro-pyridin-3-yl)-phenyl]-ethyl}-phenyl)-methanesulfonamide (88) as a solid.

1. temperatureThe reaction mixture was cooled to RT
2. extractionextracted with EtOAc
3. washThe organic layer was washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe crude residue was purified by SiO2 chromatography
7. washeluted with 10% MeOH/DCM