反应详情

温度

120 °C

To a solution of 2-Nitrophenylpyruvic acid (1.3 g, 6.22 mmol) in dry dioxane 12 mL was added morpholine (1.5 ml, 17.23 mmol) and a catalytical quantity of p-TSA. Then the resulting mixture was firstly sonicated and then heated in microwave conditions at 120° C. for 30 min. Dioxane was evaporated at reduced pressure and the crude vigourously stirred in 1/1 EtOAc/H2O (10 mL) overnight. The organic layer was separated and the aqueous phase washed with EtOAc (×2). The combined organic layer was dried over Na2SO4 anhydrous and solvent was removed at reduced pressure. Finally, the crude product was purified by flash chromatography on silica (ETP to 1:1 ETP/EtOAc) to obtain the titled compound (3.34 g, yield 64%).

1. customThen the resulting mixture was firstly sonicated
2. customDioxane was evaporated at reduced pressure
3. customThe organic layer was separated
4. washthe aqueous phase washed with EtOAc (×2)
5. dry with materialThe combined organic layer was dried over Na2SO4 anhydrous and solvent
6. customwas removed at reduced pressure
7. customFinally, the crude product was purified by flash chromatography on silica (ETP to 1:1 ETP/EtOAc)