反应详情

The product of Example 19D (371 mg, 0.5954 mmol), ammonium chloride (208.6 mg, 3.900 mmol), and iron powder (204.5 mg, 3.662 mmol) in a mixture of water (6 mL), ethanol (12 mL) and tetrahydrofuran (12 mL) was heated at 90° under a nitrogen atmosphere for 3 hours. The reaction was cooled to room temperature, diluted with ethyl acetate (200 mL), and washed with water (2×50 mL) and brine (50 mL). The organic was dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation in vacuo to give the product as an off-white solid (321 mg, 91%).

1. temperaturewas heated at 90° under a nitrogen atmosphere for 3 hours
2. washwashed with water (2×50 mL) and brine (50 mL)
3. dry with materialThe organic was dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporation in vacuo