反应详情

To a solution of 632 (ca. 386 mM) in 1,4-dioxane was added 2,3-dichloro-5,6-dicyanobenzoquinone (83.8 g, 502 mM) followed by water (final 4.8%). The resulting mixture was stirred 2 hours at room temperature and then quenched with one volume of saturated sodium bicarbonate. The mixture was evaporated in vacuo to remove 1,4-dioxane and extracted 3× with ethyl acetate. The combined organic layers were dried over sodium sulfate and evaporated in vacuo to give a crude solid that was purified on a silica-gel column with 94:5:1 dichloromethane/methanol/ammonium hydroxide as eluent to give P-0956 (approximately 50% yield for 3 steps) as a white solid.

1. customquenched with one volume of saturated sodium bicarbonate
2. customThe mixture was evaporated in vacuo
3. customto remove 1,4-dioxane
4. extractionextracted 3× with ethyl acetate
5. dry with materialThe combined organic layers were dried over sodium sulfate
6. customevaporated in vacuo
7. customto give a crude solid that
8. customwas purified on a silica-gel column with 94:5:1 dichloromethane/methanol/ammonium hydroxide as eluent
9. customto give P-0956 (approximately 50% yield for 3 steps) as a white solid