反应详情

温度

90 °C

The product from Example 13A (0.578 g, 1.26 mmol), iron (0.352 g, 6.31 mmol), and ammonium chloride (0.101 g, 1.89 mmol) were combined in a mixture of tetrahydrofuran (9 mL), ethanol (9 mL), water (3 mL) and heated at 90° C. for 2 hours. The mixture was cooled, filtered through Celite and the Celite pad was washed repeatedly with methanol. The filtrate was concentrated and the residue was partitioned between ethyl acetate and water. The organic layer was washed with saturated aqueous sodium chloride, dried (anhydrous Na2SO4), filtered, and concentrated to afford the title compound (0.52 g, 96%).

1. temperatureThe mixture was cooled
2. filtrationfiltered through Celite
3. washthe Celite pad was washed repeatedly with methanol
4. concentrationThe filtrate was concentrated
5. customthe residue was partitioned between ethyl acetate and water
6. washThe organic layer was washed with saturated aqueous sodium chloride
7. dry with materialdried (anhydrous Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated