反应详情

To a cooled (0° C.) solution of 1-acetylpiperidin-4-ol (2.0 g, 14.2 mmol) in DMF (25 mL) is added sodium hydride (60% dispersion in mineral oil, 567 mg, 14.2 mmol). After stifling at 0° C. for 15 min, 3-bromo-5-bromomethyl-pyridine (2.4 g, 9.45 mmol) is added. The reaction is allowed to warm and stir at room temperature for 1 h. The reaction is quenched with the addition of saturated aqueous ammonium chloride and water and is extracted with EtOAc. The combined organic layers are dried (Na2SO4) and concentrated. The crude product is purified by silica gel column (0-10% MeOH in DCM) to provide the title compound (2.1 g).

1. temperatureto warm
2. customThe reaction is quenched with the addition of saturated aqueous ammonium chloride and water
3. extractionis extracted with EtOAc
4. dry with materialThe combined organic layers are dried (Na2SO4)
5. concentrationconcentrated
6. customThe crude product is purified by silica gel column (0-10% MeOH in DCM)