反应详情

温度

80 °C

The product of Example 224D (174 mg, 0.2868 mmol), ammonium chloride (100.5 mg, 1.879 mmol), and iron powder (98.5 mg, 1.764 mmol) in a mixture of water (3 mL), ethanol (6 mL) and tetrahydrofuran (6 mL) was heated at 80° C. under a nitrogen atmosphere for 1 hour. The reaction was cooled to room temperature, diluted with ethyl acetate (100 mL), and washed with water (2×25 mL) and brine (25 mL). The organic was dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation in vacuo to give the product as a yellow solid (160 mg, 97%).

1. temperatureThe reaction was cooled to room temperature
2. washwashed with water (2×25 mL) and brine (25 mL)
3. dry with materialThe organic was dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporation in vacuo