反应详情

1 N Sodium Hydroxide (2 mL) was added to a solution of 30 (94 mg, 0.15 mmol, 1 equiv) in CH2Cl2 (2 mL) and the reaction mixture was stirred at RT for 3 days. The reaction was then acidified to pH 2 with 1 N HCl and the product extracted into CH2Cl2 (100 mL). The organic layer was washed with saturated aqueous NaHCO3 (2×50 mL), dried over MgSO4, filtered and concentrated to dryness. The residue was purified by silica gel flash column chomatography (20% EtOAc in hexanes) to provide 31 (47 mg, 64%) as a yellow oil. 1HNMR (400 MHz, DMSO-d6): δ 11.52 (br s, 1H), 7.69 (m, 1H), 7.57 (m, 1H), 7.34-7.21 (m, 4H), 7.15 (m, 2H), 7.07 (m, 1H), 6.99 (m, 2H), 6.59 (m, 2H), 3.86 (s, 3H), 2.16 (s, 3H). MS m/z 486.1 (M−H)−.

1. extractionthe product extracted into CH2Cl2 (100 mL)
2. washThe organic layer was washed with saturated aqueous NaHCO3 (2×50 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. customThe residue was purified by silica gel flash column chomatography (20% EtOAc in hexanes)