反应详情

温度

65 °C

To a stirred solution of 1-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)ethan-1-one oxime (5.55 g, 18.36 mmol) in acetic acid (40 mL) was added zinc dust (6.00 g, 91.79 mmol). The resulting mixture was heated to 65° C. After 1 h, the mixture was allowed to cool to room temperature and was filtered through Celite. The filtercake was washed with methanol (100 mL). The filtrate was concentrated, and the residue dissolved in 5N ammonium hydroxide solution (75 mL). The mixture was extracted with chloroform (2×50 mL). The combined organic phases were dried over magnesium sulfate, filtered, and concentrated to provide 4.56 g (86%) of 1-(3-methoxy-4-((6-methoxypyridin-3-yl)methoxy)phenyl)ethan-1-amine as a yellow oil.

1. temperatureto cool to room temperature
2. filtrationwas filtered through Celite
3. washThe filtercake was washed with methanol (100 mL)
4. concentrationThe filtrate was concentrated
5. dissolutionthe residue dissolved in 5N ammonium hydroxide solution (75 mL)
6. extractionThe mixture was extracted with chloroform (2×50 mL)
7. dry with materialThe combined organic phases were dried over magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated