反应详情

A solution of the product of Example 9D (1.06 g, 2.76 mmol), iron powder (0.63 g, 11.04 mmol) and ammonium chloride (0.18 g, 3.31 mmol) in a methanol (18 mL), tetrahydrofuran (18 mL), and water (6 mL) solution was heated to reflux for 3 hours. The resultant mixture was diluted with methanol (50 mL) and filtered through a pad of celite. The filtrate was concentrated under vacuum to a volume of 10 mL, the solution diluted with water (50 mL) and extracted with ethyl acetate (2×50 mL). The combined extracts were dried over magnesium sulfate, filtered and concentrated under vacuum to provide the title compound (0.99 g, 100%).

1. temperatureto reflux for 3 hours
2. filtrationfiltered through a pad of celite
3. concentrationThe filtrate was concentrated under vacuum to a volume of 10 mL
4. additionthe solution diluted with water (50 mL)
5. extractionextracted with ethyl acetate (2×50 mL)
6. dry with materialThe combined extracts were dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under vacuum