反应详情

温度

70 °C

step 3—A mixture of 22 (82 mg, 0.267 mmol), 48% HBr (90 □L, 0.784 mmol) and HOAc (4 mL) in a sealed tube was heated overnight at 70° C. The reaction mixture was carefully poured into a cold sat'd. aq. NaHCO3 solution, and then extracted with EtOAc. The organic layer was washed with brine dried (Na2SO4), filtered and concentrated. The crude residue was purified by preparative TLC plate developed with 66% EtOAc in hexanes to afford 39 mg (50% yield) of 1-6 as a light yellow solid.

1. additionThe reaction mixture was carefully poured into a cold sat'd
2. extractionaq. NaHCO3 solution, and then extracted with EtOAc
3. washThe organic layer was washed with brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude residue was purified by preparative TLC plate