反应详情

The product (1.00 g, 3.48 mmol) from Step A was added to a solution of potassium hydroxide (1.0 g) in 30 mL of absolute ethanol. The mixture was warmed to reflux and, after 5 h, cooled to room temperature. The solution was then acidified with glacial acetic acid, and concentrated under reduced pressure. The product was extracted into ethyl acetate, and the combined ethyl acetate extracts were washed sequentially with water and saturated aqueous brine, dried (magnesium sulfate) and concentrated to give the crude product as an orange semisolid. Purification by flash chromatography (silica gel, 15% ethyl acetate-hexanes) afforded the product as an off-white, sticky foam. LC/MS 316.0 (M+1).

1. temperatureThe mixture was warmed
2. temperatureto reflux and, after 5 h
3. concentrationconcentrated under reduced pressure
4. extractionThe product was extracted into ethyl acetate
5. washthe combined ethyl acetate extracts were washed sequentially with water and saturated aqueous brine
6. dry with materialdried (magnesium sulfate)
7. concentrationconcentrated