反应详情

To a stirred solution of 6-methoxy-1-[1-(1-methyl-1H-imidazole-4-sulfonyl)-piperidin-4-yl]-3,4-dihydro-isoquinoline (0.077 g, 0.197 mmol) in MeOH (3 ml) cooled to 0° C. was added NaBH4. The reaction mixture was then stirred at RT for 2 hours and diluted with water (5 ml) and sat. NaHCO3 (5 ml). The mixture was extracted with EtOAc (3×10 ml). The combined organics were washed with brine (1×10 ml), dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by radial chromatography (SiO2, 1 mm, CH2Cl2 to 5% MeOH/CH2Cl2) to give the product as an oil (0.055 g, 0.141 mmol, 71% yield).

1. extractionThe mixture was extracted with EtOAc (3×10 ml)
2. washThe combined organics were washed with brine (1×10 ml)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by radial chromatography (SiO2, 1 mm, CH2Cl2 to 5% MeOH/CH2Cl2)