反应详情

A mixture of the ester (0.4 g, 0.0009 mol) obtained from step 3, in 2N NaOH (0.9 mL) and dioxane (0.5 mL) was stirred at room temperature for 1.5 h. The resulting clear solution was diluted with water (5.0 mL), acidified with 5% citric acid and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with water (2×15 mL), dried (Na2SO4), and concentrated to afford the title compound (0.38 g) as a white powder: 1H NMR (CD3OD/400 MHz) δ 8.06 (d, 1H, J=8.0 Hz), 7.81 (s, 1H), 7.51 (m, 2H), 6.99 (m 2H), 5.64 (s, 1H), 5.48 (s, 2H), 2.50 (s, 3H), and 2.15 (s, 3H); ES-HRMS m/z 419.0892(M+H calcd for C20H17N2O4SF2 requires 419.0872).

1. extractionextracted with EtOAc (2×20 mL)
2. washThe combined organic extracts were washed with water (2×15 mL)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated