反应详情

To 1-(3-hydroxypropyl)piperidine (287 mg) are successively added sodium (46 mg) and 2-chloro-4-(4-{3-[(3S)-3-methylpiperidin-1-yl]propoxy}phenyl)pyridine (345 mg). The mixture is heated overnight, cooled back to room temperature and dissolved in dichloromethane (20 mL). The organic phase is washed with water (20 mL), dried over magnesium sulphate, concentrated under reduced pressure and purified over silica gel (eluent (dichloromethane/methanol from 100/0 to 90/10). Fraction containing the expected product are pooled and concentrated under reduced pressure. The crude base is dissolved in ethanol, oxalic acid (32 mg) is added and the precipitate that appears separated by filtration and dried to give 70 mg of 2-(3-piperidinopropoxy)-4-(4-{3-[(3S)-3-methylpiperidin-1-yl]propoxy}phenyl)pyridine, dioxalate as a white solid melting at 122° C.

1. temperatureThe mixture is heated overnight
2. washThe organic phase is washed with water (20 mL)
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated under reduced pressure
5. custompurified over silica gel (eluent (dichloromethane/methanol from 100/0 to 90/10)
6. additionFraction containing the expected product
7. concentrationconcentrated under reduced pressure
8. dissolutionThe crude base is dissolved in ethanol
9. additionoxalic acid (32 mg) is added
10. customthe precipitate that appears separated by filtration
11. customdried