反应详情

温度

40 °C

To a solution of the product from Example 63C (1.85 g, 4.80 mmol) in methanol/dichloromethane (50 mL) was added 3,5-dimethoxybenzaldehyde (0.80 g, 4.80 mmol), macroporous-cyanoborohydride resin (8.09 g, 4.80 mmol, 2.24 mol/g) and acetic acid (1.6 mL, 4.80 mmol). The reaction was stirred at 40° C. for 18 hours under an atmosphere of nitrogen. The reaction was cooled to room temperature, filtered and concentrated. Silica gel chromatography eluting with 3% methanol/dichloromethane gave the title compound. The title compound was dissolved in methanol (10 mL) and treated with HCl (1.25 M in methanol, 5.1 mL), concentrated and dried under vacuum to give the title compound as the corresponding hydrochloride salt. MS (DCI) m/z 536.3 (M+H)+.

1. temperatureThe reaction was cooled to room temperature
2. filtrationfiltered
3. concentrationconcentrated
4. washSilica gel chromatography eluting with 3% methanol/dichloromethane