反应详情

A solution of the product of Example 43A (0.73 g, 2.0 mmol), iron powder (1.12 g, 20 mmol) and ammonium chloride (1.08 g, 20 mmol) in methanol (20 mL), tetrahydrofuran (20 mL), and water (10 mL) was heated at 80° for 48 hours. After cooling to room temperature, the mixture was diluted with methanol (50 mL) and filtered through a pad of celite. The filtrate was concentrated under vacuum then purified by column chromatography on silica gel using methanol/dichloromethane as eluent to provide the title product (670 mg, 100%).

1. filtrationfiltered through a pad of celite
2. concentrationThe filtrate was concentrated under vacuum
3. customthen purified by column chromatography on silica gel