反应详情

The product from Step A (3.09 g, 9.14 mmol) was added to glacial acetic acid (250 mL). Zinc (21.68 g, 331.7 mmol) was gradually added with stirring. After stirring 1.5 hours, zinc was filtered from the mixture and the solution was concentrated to a dark oil. Methylene chloride (100 mL) was added to the oil and the desired product crystallized out overnight (0.3154 g), mp>300° C.

1. stirringAfter stirring 1.5 hours
2. filtrationzinc was filtered from the mixture
3. concentrationthe solution was concentrated to a dark oil
4. additionMethylene chloride (100 mL) was added to the oil
5. customthe desired product crystallized out overnight (0.3154 g), mp>300° C.