反应详情

温度

100 °C

4-Nitrobenzaldehyde oxime (Intermediate 3, 20 g, 120.5 mmol) and bicyclo[2.2.1]hepta-2,5-diene (32.45 ml, 3015.25 mmol) were added to THF (200 ml) followed by dropwise addition of bleach (6.15% NaOCl, 861.5 ml). The reaction was allowed to stir overnight and then the THF and H2O layers were separated, the THF layer was dried over Na2SO4 and then concentrated under vacuum. The dried material was added to dioxane and heated to 100° C. for 7 days. The crude material was purified by column chromatography using 5–50% EtOAc in hexanes to yield the final product (10 g).

1. customthe THF and H2O layers were separated
2. dry with materialthe THF layer was dried over Na2SO4
3. concentrationconcentrated under vacuum
4. additionThe dried material was added to dioxane
5. customThe crude material was purified by column chromatography