反应详情

A solution of 66D (55 mg, 0.082 mmol) in 10 mL DMF was added to a solution of PyBOP (88 mg, 0.17 mmol), DMAP (49 mg, 0.4 mmol), and TEA (40 mg, 0.4 mmol) in CH2Cl2 (30 mL) dropwise through syringe pump over 3 h. The solution was stirred at rt for 16 h. The solution washed with 1M H3PO4, sat NaHCO3 and brine, dried (Na2SO4) and concentrated. The crude product was purified by flash chromatography (0 to 80% EtOAc in hexanes) to give 66F (8.5 mg, 16%). MS (ESI) m/z 654.8 (M+H)+.

1. washThe solution washed with 1M H3PO4
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated
4. customThe crude product was purified by flash chromatography (0 to 80% EtOAc in hexanes)