反应详情

EDAC.HCl (114 mg, 0.59 mmol) was added to a mixture of compound 91C (125 mg, 0.59 mmol), propylamine (49 μL, 0.59 mmol) and HOBT (80 mg, 0.59 mmol) in 1 mL of CH3CN. The reaction was stirred for 72 hours. After this time, the mixture was diluted with AcOEt. The organic layer was washed three times with HCl 2N, three times with NaOH 2N, dried over MgSO4 and concentrated. A with solid was obtained (100 mg, 67%). NMR 1H (ppm, CDCl3): 7.57 (d., J3=7.05 Hz, 2H), 7.52-7.32 (m, 6H), 7.23 J3=7.94 Hz, 1H), 5.65 (br. s., 1H), 3.62 (s, 2H), 3.20-3.13 (m, 2H), 1.44 (sex. J3=7.21 Hz, 2H), 0.83 (t, J3=7.43 Hz, 3H). NMR 13C (ppm, CDCl3): 170.9, 141.9, 140.5, 135.5, 129.3, 128.8, 128.2, 127.5, 127.0, 126.0, 43.8, 41.3, 22.7, 11.2. MS (+ESI): M+H+: 254.3.

1. washThe organic layer was washed three times with HCl 2N, three times with NaOH 2N
2. dry with materialdried over MgSO4
3. concentrationconcentrated
4. customA with solid was obtained (100 mg, 67%)