反应详情

温度

90 °C

The product of Example 154A (307 mg, 0.463 mmol), ammonium chloride (162 mg, 3.03 mmol), and iron powder (159 mg, 2.845 mmol) in a mixture of water (3 mL), ethanol (6 mL) and tetrahydrofuran (6 mL) was heated at 90° 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 (3×50 mL) and brine (50 mL). The organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated by rotary evaporation in vacuo to give the product as a light yellow solid (224 mg, 76

1. temperatureThe reaction was cooled to room temperature
2. washwashed with water (3×50 mL) and brine (50 mL)
3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporation in vacuo