反应详情

温度

0 °C

To a solution of 28c (311 mg, 0.532 mmol) in 5 mL THF/H2O (4:1) at 0° C., were added 30% H2O2 (0.241 mL, 2.13 mmol) and IM LiOH (0.851 mL, 0.851 mmol). The mixture was stirred at 0° C. for 2 h, then Na2SO3 and 10 mL H2O were added. The organic solvent was evaporated under a stream of nitrogen. The precipitate was filtered and rinsed with H2O and 0.1 N NaOH. The combined aqueous filtrate was acidified with conc. HCl, then extracted with EtOAc (3×). The combined organic extract was washed with brine, dried (Na2SO4), and concentrated to afford 208 mg (96%) of 28d. MS (ESI) 410.3 (M+H+), 432.3 (M+Na+), 408.2 (M−H+).

1. customThe organic solvent was evaporated under a stream of nitrogen
2. filtrationThe precipitate was filtered
3. washrinsed with H2O and 0.1 N NaOH
4. extractionextracted with EtOAc (3×)
5. extractionThe combined organic extract
6. washwas washed with brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated