反应详情

A mixture of 106a (330 mg, 0.47 mmol) and LiOH.H2O (196 mg, 4.67 mmol) in THF/i-PrOH/water (5.0 mL/3.0 mL/2.0 mL) was stirred at rt for 1 h. The mixture was extracted with EA. The combined organic layers were dried over Na2SO4, filtered and concentrated. The residue was purified by prep-HPLC to give 106 (30 mg, 8% for two steps) as white solid. 1H NMR (500 MHz, CDCl3): δ 8.52 (s, 1H), 8.26 (s, 1H), 7.52 (t, J=8.0 Hz, 1H), 7.45 (s, 1H), 7.13-7.10 (m, 1H), 6.69 (s, 1H), 6.52 (d, J=8.0 Hz, 1H), 6.22 (d, J=8.5 Hz, 1H), 4.34 (s, 2H), 4.27 (t, J=5.0 Hz, 2H), 2.98-2.97 (m, 2H), 2.87-2.85 (m, 2H), 1.99-1.96 (m, 4H), 1.86 (s, 3H). ESI-LCMS: m/z=655 [C34H31FN6O5S+H]+

1. extractionThe mixture was extracted with EA
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by prep-HPLC