反应详情

To a solution of the product from Example 74A (1.64 g, 5.32 mmol), iron powder (1.49 g, 26.62 mmol) and ammonium chloride (430 mg, 7.98 mmol) in a mixture of tetrahydrofuran (20 mL), water (6 mL) and ethanol (20 mL) was heated to reflux for 3 hours. The mixture was cooled to room temperature, filtered through a pad of celite, which was washed with ethanol and the resultant filtrate concentrated under vacuum. The material was then dissolved in water (50 mL) and extracted with ethyl acetate (50 mL), the organic layer dried and concentrated under vacuum to provide the title compound as a yellow oil (1.43 g, 97%).

1. temperaturewas heated
2. temperatureto reflux for 3 hours
3. filtrationfiltered through a pad of celite, which
4. washwas washed with ethanol
5. concentrationthe resultant filtrate concentrated under vacuum
6. dissolutionThe material was then dissolved in water (50 mL)
7. extractionextracted with ethyl acetate (50 mL)
8. customthe organic layer dried
9. concentrationconcentrated under vacuum