反应详情

温度

70 °C

To a solution of 302b (1.8 g, 7.96 mmol) in ethanol (20 mL) and water (20 mL), NH4Cl (3.3 g, 63.6 mmol) and iron powder (1.80 g, 31.8 mmol) were added. The reaction mixture was heated at 70° C. for 2 h. After that, the mixture was cooled to room temperature and filtered. The filtrate was evaporated and the residue was extracted with methylene chloride (3×30 mL), dried Na2SO4, and concentrated to afford the crude product, which was purified on flash column eluting with 50:1 methylene chloride/methanol containing 0.5% triethylamine to afford 302c as a yellow oil (1.3 g, 83%). LCMS: (M+H)+ 197

1. temperatureAfter that, the mixture was cooled to room temperature
2. filtrationfiltered
3. customThe filtrate was evaporated
4. extractionthe residue was extracted with methylene chloride (3×30 mL), dried Na2SO4
5. concentrationconcentrated
6. customto afford the crude product, which
7. customwas purified on flash column
8. washeluting with 50:1 methylene chloride/methanol containing 0.5% triethylamine