反应详情

step 2—A solution of 126 (156 mg, 0.471 mmol), 48% HBr (150 □L, 1.30 mmol) and HOAc (4 mL) in 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 (Na2SO4), filtered and concentrated. The crude residue was purified on a preparative SiO2 TLC plate developed with 66% EtOAc/hexanes to afford 124 mg (83%) of I-46 as a white solid.

1. extractionextracted with EtOAc
2. washThe organic layer was washed with brine
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude residue was purified on a preparative SiO2 TLC plate
7. customto afford 124 mg (83%) of I-46 as a white solid