反应详情

温度

80 °C

A suspension of the product of Example 199B (282 mg, 0.5816 mmol), iron powder (200 mg, 3.577 mmol), and ammonium chloride (204 mg, 3.809 mmol) in ethanol (8 mL) and water (4 mL) was heated at 80° C. for 45 minutes. After cooling to room temperature, the mixture was diluted with ethyl acetate (100 mL) and washed with water (2×50 mL) and brine (50 mL). The organic phase was dried over sodium sulfate, filtered and concentrated under vacuum to provide the title compound as a beige solid (250 mg, 94%).

1. temperatureAfter cooling to room temperature
2. washwashed with water (2×50 mL) and brine (50 mL)
3. dry with materialThe organic phase was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated under vacuum