反应详情

A mixture of Example 96F (0.95 g, 3.5 mmol), iron (0.78 g, 13.9 mmol), and NH4Cl (0.19 g, 3.5 mmol) in 9:1 ethanol/water (80 mL) was heated to 60° C. for 4 hours, cooled to room temperature, and filtered through a pad of diatomaceous earth (Celite®). The pad was washed with THF and the filtrate was concentrated. The concentrate was suspended in water and filtered. The filter cake was washed with water and dried to provide 0.82 g (97% yield) of the desired product.

1. filtrationfiltered through a pad of diatomaceous earth (Celite®)
2. washThe pad was washed with THF
3. concentrationthe filtrate was concentrated
4. filtrationfiltered
5. washThe filter cake was washed with water
6. customdried