反应详情

A solution of the product of Example 38a (2.7 g, 8.97 mmol), iron powder (2.0 g, 35.9 mmol) and ammonium chloride (0.58 g, 10.76 mmol) in a methanol (6 mL), THF (6 mL), and water (2 mL) solution was heated to reflux for 1.5 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 washed with 10% sodium chloride then dried over magnesium sulfate, filtered and concentrated under vacuum to provide the title compound (2.46 g, 77%).

1. temperatureto reflux for 1.5 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. washThe combined extracts were washed with 10% sodium chloride
7. dry with materialthen dried over magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated under vacuum