反应详情

A solution of 1E (27 mg, 0.04 mmol) in CH2Cl2 (2 mL) at 0° C. was treated with TFA (100 μL). The reaction was warmed to room temperature and stirred for three hours. The mixture was poured into EtOAc:buffer (1:1, pH 7, 40 mL) and the layers were separated. The organic layer was washed with pH 7 buffer (1×10 mL), dried (Na2SO4), filtered and concentrated to a yellow oil. The crude product was purified by preparative HPLC to afford 1F as a white solid (19 mg, 88%). 1H NMR (Acetone-d6) δ 8.80 (d, 1H, J=7.5 Hz), 8.17 (brs 1H), 8.01 (d, 1H, J=1.8 Hz), 7.81 (d, 1H, J=7.0 Hz), 7.45 (d, 1H, J=1.8 Hz), 7.36 (m, 2H), 7.15 (m, 5H), 6.97 (d, 1H, J=6.6 Hz), 6.89 (d, 1H, J=7.0 Hz), 6.79 (t, 1H, J=7.8 Hz), 3.77 (s, 3H), 3.64 (q, 2H, J=5.28 Hz), 2.93 (t, 2H, J=5.24 Hz). HPLC retention time=3.297 min. (YMC S5 ODS 4.6×50 mm, 10-90% aqueous methanol containing 0.2% H3PO4, 4 min gradient, monitored at 220 nm). m/z=516.9 (M+H+).

1. custombuffer (1:1, pH 7, 40 mL) and the layers were separated
2. washThe organic layer was washed with pH 7 buffer (1×10 mL)
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated to a yellow oil
6. customThe crude product was purified by preparative HPLC