反应详情

To a solution of 76B (209 mg, 0.54 mmol) in THF (5 mL) at 0° C., was added H2O2 (0.33 mL, 50%, 5.4 mmol) dropwise, followed by aq. LiOH (1.1 mL, 1.0 M, 1.1 mmol). The solution was stirred at rt for 2 h. Aq. Na2SO3 (1M, 20 mL) was added and stirred rt for 30 min. The aqueous phase was extracted with CH2Cl2 (2×10 mL), acidified to pH=2 with 1N HCl, and extracted with EtOAc (3×20 mL). The organic layer washed with brine, dried (Na2SO4) and concentrated to give 76C (110 mg, 90%). MS (ESI) m/z 229.0 (M+H)+.

1. stirringstirred rt for 30 min
2. extractionThe aqueous phase was extracted with CH2Cl2 (2×10 mL)
3. extractionextracted with EtOAc (3×20 mL)
4. washThe organic layer washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated