反应详情

The product from Example 268B (6.0 g, 10 mmol), iron powder (2.8 g, 50 mmol) and ammonium chloride (0.81 g, 15 mmol) in a mixture of ethanol (60 mL), tetrahydrofuran (60 mL), and water (20 mL) was heated under reflux for 5 hours and then cooled to room temperature. The reaction mixture was filtered through Celite and the filter pad was rinsed with ethanol (100 mL). The filtrate was evaporated under reduced pressure to leave a residue which was triturated with hexanes/ethyl acetate 4/1 to provide the title product (2.39 g, 42%) as a tan solid.

1. temperaturewas heated
2. temperatureunder reflux for 5 hours
3. filtrationThe reaction mixture was filtered through Celite
4. washthe filter pad was rinsed with ethanol (100 mL)
5. customThe filtrate was evaporated under reduced pressure
6. customto leave a residue which
7. customwas triturated with hexanes/ethyl acetate 4/1