反应详情

To a stirred solution of tert-butyl 3-methoxy-4-((6-methylpyridin-3-yl)methoxy)benzylcarbamate (29.74 g, 82.97 mmol) in dichloromethane (100 mL) was added trifluoroacetic acid (50 mL, 649.0 mmol). The resulting brown 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 (3×100 mL). The combined organic phases were dried over magnesium sulfate, filtered, and concentrated to provide 19.22 g (90%) of (3-methoxy-4-((6-methylpyridin-3-yl)methoxy)phenyl)methanamine as brown 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 (3×100 mL)
5. dry with materialThe combined organic phases were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated