反应详情

To a stirred solution of tert-butyl 3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)benzylcarbamate (31.92 g, 85.25 mmol) in dichloromethane (100 mL) was added trifluoroacetic acid (75 mL, 973.5 mmol). The resulting yellow solution was allowed to stir at room temperature. After 2 h, the reaction mixture was concentrated to dryness, and the residue was dissolved in water (250 mL). The acidic solution was extracted with diethyl ether (2×125 mL; organic phases discarded). The aqueous phase was then made basic with concentrated ammonium hydroxide. The basic aqueous phase was then extracted with dichloromethane (2×200 mL). The combined organic phases were dried over magnesium sulfate, filtered, and concentrated to provide 21.46 g (92%) of (3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)methanamine as an off-white solid.

1. concentrationthe reaction mixture was concentrated to dryness
2. dissolutionthe residue was dissolved in water (250 mL)
3. extractionThe acidic solution was extracted with diethyl ether (2×125 mL; organic phases discarded)
4. extractionThe basic aqueous phase was then extracted with dichloromethane (2×200 mL)
5. dry with materialThe combined organic phases were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated