反应详情

A solution of 77G (170mg, 0.34 mmol) in 5% TFA/DCM (5 mL) was stirred at rt for 5 h and LC-MS showed completion. The mixture was concentrated and the residue was dissolved in EtOAc (30 mL), washed with saturated sodium bicarbonate solution (15 mL), brine (10 mL), dried (MgSO4) and evaporated to give desired product 77H (121 m, 89%) as a white solid: Rf (10% MeOH/DCM) 0.39; HPLC (Phenomenex Luna 5 u C18 4.6×50 mm, linear gradient over 4 min) retention time 3.2 min (100%); MS (ES) m/z 344.1 [M+H]+; HRMS calcd for C20H33N3OSiCl 394.2081, Found 394.2080.

1. concentrationThe mixture was concentrated
2. dissolutionthe residue was dissolved in EtOAc (30 mL)
3. washwashed with saturated sodium bicarbonate solution (15 mL), brine (10 mL)
4. dry with materialdried (MgSO4)
5. customevaporated