反应详情

A mixture of the product of Example 364C (1.63 g, 2.63 mmol), iron powder (0.737 g, 13.1 mmol, 5 equiv., from Acros, electrolytically reduced, reagent, powder), and ammonium chloride (0.211 g, 3.94 mmol, 1.5 equiv.) in tetrahydrofuran/ethanol/water (30/30/10 mL) was heated under reflux for 2.5 hours. The reaction mixture was cooled to room temperature and filtered through Celite, rinsing the Celite pad with 50 mL of ethanol. The resulting filtrate was evaporated under reduced pressure and the residue was partitioned between ethyl acetate (100 mL) and water (100 mL). The aqueous phase was washed with ethyl acetate (2×100 mL). The combined organic phases were washed with brine (50 mL), dried over anhydrous magnesium sulfate, filtered, and evaporated under reduced pressure to give the title compound (1.48 g, 95%) as a faintly yellow solid.

1. temperatureunder reflux for 2.5 hours
2. filtrationfiltered through Celite
3. washrinsing the Celite pad with 50 mL of ethanol
4. customThe resulting filtrate was evaporated under reduced pressure
5. customthe residue was partitioned between ethyl acetate (100 mL) and water (100 mL)
6. washThe aqueous phase was washed with ethyl acetate (2×100 mL)
7. washThe combined organic phases were washed with brine (50 mL)
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationfiltered
10. customevaporated under reduced pressure