反应详情

To a suspension of sodium hydride (60% in mineral oil, 1.07 g, 26.8 mmol) in dry DMF (20 mL) at room temperature under nitrogen, Intermediate 5b (1.89 g, 11.6 mmol) was added portionwise over 2 min, and the resulting brown solution was stirred for 20 min. Intermediate 1f (1.60 g, 8.93 mmol) was added, and the solution stirred at 60° C. for 2 h. The dark brown solution was cooled to room temperature and concentrated under vacuum. The residue was purified by SCX-2, washing with MeOH (200 mL) and eluting with 2M NH3 in MeOH, to leave a dark brown foam (3.21 g). Further purification by FCC, using 2-10% [2M NH3 in MeOH] in DCM, gave a brown foam (2.11 g, 76%). 1H NMR (400 MHz, d6-DMSO): 1.37 (3H, d), 1.39 (3H, d), 1.59 (1H, m), 1.91 (1H, m), 2.11 (1H, m), 2.33 (1H, m), 3.58 (1H, sept), 3.96 (1H, dd), 5.55 (1H, dd), 7.18-7.37 (4H, m), 7.51 (1H, d), 7.68 (1H, d), 8.20 (1H, d).

1. stirringthe solution stirred at 60° C. for 2 h
2. concentrationconcentrated under vacuum
3. customThe residue was purified by SCX-2
4. washwashing with MeOH (200 mL)
5. washeluting with 2M NH3 in MeOH