反应详情

温度

80 °C

To a solution of the product from Step 1 (5.34 g) in dioxane (25 ml) was added acetic anhydride (6 ml) and pyridine (4 ml). After 60 hours of stirring at 80° C., the solution was concentrated under reduced pressure and the residue was dissolved into ethyl acetate. The organic layer was washed with 2M sodium carbonate, 10% aqueous HCl, water and brine, dried over sodium sulfate and evaporated. The product was purified by flash chromatography (ISCO, 5%-20% ethyl acetate in hexanes) to provide a beige solid (5.27 g). LRMS (ES+) m/z 262.0 (M+H)+.

1. concentrationthe solution was concentrated under reduced pressure
2. dissolutionthe residue was dissolved into ethyl acetate
3. washThe organic layer was washed with 2M sodium carbonate, 10% aqueous HCl, water and brine
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customThe product was purified by flash chromatography (ISCO, 5%-20% ethyl acetate in hexanes)