反应详情

A mixture of 438 (451 mg, 1.14 mmol) and 1-methylpiperazine (152 μL, 137 mg, 1. 37 mmol) in DCM (7 mL) was stirred at room temperature for 10 min. It was then treated with NaBH(OAc)3 (340 mg, 1.60 mmol) and stirred at room temperature overnight. The reaction mixture was the diluted with DCM (20 mL) and washed with saturated NaHCO3 solution (20 mL). It was then dried over anhydrous Na2SO4, filtered and concentrated. The residue was purified by flash chromatography using the gradient 30-50% MeOH (with 2% Et3N) in EtOAc as an eluent, yielding 439 of (308 mg, 52% yield). LCMS: (M+H) 480.0 (100%).

1. stirringstirred at room temperature overnight
2. washwashed with saturated NaHCO3 solution (20 mL)
3. dry with materialIt was then dried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by flash chromatography