反应详情

To a solution compound 84A (50 mg, 0.136 mmol) in DMF (5 ml) was added sodium hydride (27.2 mg, 0.680 mmol)(60%). The reaction mixture was stirred for 10 min and compound 2C (77 mg, 0.122 mmol) was added. The resulting mixture was stirred for 1 hour and methanol (3 ml), 10% NaOH and water (1 ml) were added. The mixture was stirred overnight, acidified with TFA and concentrated. The residue was dissolved in a mixture of DMSO-methanol and purified by reverse phase HPLC (mobile phase: 0%-60% acetonitrile in 0.1% TFA aqueous solution during 60 min) to provide the title compound 91 as a TFA salt: 1H NMR (500 MHz, PYRIDINE-D5) δ ppm 8.62 (1H, s), 8.41 (1H, s), 8.35 (2H, d), 7.94 (1H, d), 7.89 (1H, d), 7.77-7.81 (1H, m), 7.43 (1H, t), 7.24-7.33 (5H, m), 5.15 (2H, s), 3.93-4.01 (2H, m), 3.87 (2H, d), 3.81 (2H, t), 3.45 (2H, t), 2.92 (2H, t), 2.79-2.85 (4H, m), 2.62-2.69 (4H, m), 2.42-2.47 (5H, m), 2.18-2.28 (2H, m), 1.89-1.98 (2H, m); LCMS (APCI) m/e 844 (M+H).

1. stirringThe resulting mixture was stirred for 1 hour
2. stirringThe mixture was stirred overnight
3. concentrationconcentrated
4. dissolutionThe residue was dissolved in a mixture of DMSO-methanol
5. custompurified by reverse phase HPLC (mobile phase: 0%-60% acetonitrile in 0.1% TFA aqueous solution during 60 min)