反应详情

3-Ethyl-3-(3-methoxy-phenyl)-azepan-2-one (as described in Step H above) (1.05 g, 4.24 mmol) in anhydrous THF (4.2 mL) was added to a solution of LiAlH4 (0.193 g, 5.09 mmol) in anhydrous THF (4.2 mL) and refluxed for 24 h. The solution was cooled, quenched with H2O (0.18 mL), 15% NaOH (0.18 mL), H2O (0.54 mL), filtered and concentrated. The residue was purified using reverse phase chromatography (95/5-5/95 H2O/CH3CN with 0.1% TFA, flow =65 mL/min) and converted to its free base using saturated NaHCO3 solution, extracted with CH2Cl2 (3×) and dried (MgSO4) to give the title compound.

1. temperaturerefluxed for 24 h
2. temperatureThe solution was cooled
3. customquenched with H2O (0.18 mL), 15% NaOH (0.18 mL), H2O (0.54 mL)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified
7. extractionextracted with CH2Cl2 (3×)
8. dry with materialdried (MgSO4)