反应详情

To a solution of compound 60b (55.0 mg, 0.102 mmol) in DCM (2 mL) at RT was added TFA (500 μL, 6.53 mmol). After stirring at rt for 0.5 h, the mixture was concentrated in vacuo and the residue was purified by flash column chromatography on silica gel (0:1-1:9 MeOH-DCM) to afford the title compound 79 (with 1.1 eq TFA) as a white solid. 1H-NMR (CDCl3; 400 MHz) δ: 8.03 (d, J=8.6 Hz, 2H), 8.00 (d, J=5.6 Hz, 1H), 7.64 (d, J=8.1 Hz, 1H), 7.56-7.62 (m, 2H), 7.15 (d, J=8.1 Hz, 1H), 6.11 (d, J=5.6 Hz, 1H), 3.87-4.05 (m, 8H), 3.57 (t, J=7.1 Hz, 2H), 3.34-3.43 (m, 2H), 3.07-3.18 (m, 2H), 2.71-2.83 (m, 2H), 1.77-1.95 (m, 4H). Mass spectrum (ESI, m/z): Calcd. for C28H29N5O3, 484.2 (M+H). found 484.5.

1. concentrationthe mixture was concentrated in vacuo
2. customthe residue was purified by flash column chromatography on silica gel (0:1-1:9 MeOH-DCM)