反应详情

温度

85 °C

In a flask equipped with a reflux condenser, the compound obtained in Example 6 1.60 g (3.77 mmol), reduced iron powder 1.05 g (18.85 mmol, 5 eq), glacial acetic acid (2 mL) and methanol (40 mL) were mixed. The mixture was refluxed in an oil bath at a temperature of 85° C. for 2.5 h. Then the iron powder was filtered of, the filtrate was diluted with ethyl acetate, washed sequentially with NaHCO3 solution and water. The organic phase was dried and concentrated to obtain yellow solid, which was identified as the title compound. Yield: 61%.

1. customIn a flask equipped with a reflux condenser
2. filtrationThen the iron powder was filtered of, the filtrate
3. additionwas diluted with ethyl acetate
4. washwashed sequentially with NaHCO3 solution and water
5. customThe organic phase was dried
6. concentrationconcentrated
7. customto obtain yellow solid, which