反应详情

To a solution of the amine 9 (80 mg, 0.235 mmol), acid 31 (47 mg, 0.235 mmol), and BOP (114.6 mg, 0.254 mmol) in DMF (2.4 mL), DIPEA (0.164 mL, 0.941 mmol) was added and the mixture was stirred for 2 h at room temperature. The reaction mixture was diluted with EtOAc (100 mL), water (50 mL) was added and the mixture filtered through paper filter. The organic phase was separated, washed with water (50 mL), brine (20 mL), dried (anhydrous Na2SO4) and concentrated under reduced pressure. The residue was purified by flash chromatography (eluent EtOAc/MeOH 10:1) to afford the title compound 32 (36.2 mg, 30% yield) as a creamy solid. 1H NMR (DMSO-d6) δ (ppm): 10.29 (s, 1H), 8.49 (d, J=5.5 Hz, 1H), 7.87 (s, 1H), 7.77 (d, J=12.7 Hz, 1H), 7.46-7.30 (m, 8H), 7.03 (s, 1H), 6.66 (d, J=5.5 Hz, 1H), 3.98 (s, 3H), 3.22 (s, 2H), 2.52 (3H, s). MS (m/z): 516.3 (M+H).

1. additionwas added
2. filtrationthe mixture filtered through paper
3. filtrationfilter
4. customThe organic phase was separated
5. washwashed with water (50 mL), brine (20 mL)
6. dry with materialdried (anhydrous Na2SO4)
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by flash chromatography (eluent EtOAc/MeOH 10:1)