反应详情

To a solution of 2-(3,4-dihydro-1H-isoquinolin-2-yl)ethylamine (36) (0.36 g, 2.0 mmol) in dichloromethane (4 mL) was added the bromide 35 (0.75 g, 2.6 mmol) in dichloromethane (5 mL) at 0° C. The mixture was allowed to warm to room temperature and stirred for 16 hours before it was poured into saturated NaHCO3 (aq. 50 mL) and extracted with dichloromethane (2×50 mL). The combined organic layers were washed with water (70 mL), brine (70 mL), dried over MgSO4, and concentrated on a rotavap. The residue was chromatographed on silica gel eluting with 3:1 to 1:1 hexanes/EtOAc to give 37 (0.39 g, 57%).

1. extractionextracted with dichloromethane (2×50 mL)
2. washThe combined organic layers were washed with water (70 mL), brine (70 mL)
3. dry with materialdried over MgSO4
4. concentrationconcentrated on a rotavap
5. customThe residue was chromatographed on silica gel eluting with 3:1 to 1:1 hexanes/EtOAc