反应详情

温度

110 °C

To a round bottom flask was added 4-(3-benzyloxy-4-methoxyphenyl)-pyrrolidin-2-one (1.76 g, 5.9 mmol), 3-iodonitrobenzene (2.64 g, 10.6 mmol), K3PO4 (2.79 g, 13 mmol), trans-cyclohexanediamine (50 μL), DMF (8 mL) and dioxane (8 mL). The mixture was stirred under N2 for 5 min before the addition of CuI (150 mg). After heating to 110° C. for 20 h, the mixture was cooled to r.t. After filtration, the reaction mixture was diluted with EtOAc (100 mL), washed with saturated NH4Cl, brine and dried over Na2SO4. Concentration and purification by column chromatography on silica gel (EtOAc:hexane=1:3) gave 1.4 g of the desired product. Yield: 57%.

1. temperaturethe mixture was cooled to r.t
2. filtrationAfter filtration
3. additionthe reaction mixture was diluted with EtOAc (100 mL)
4. washwashed with saturated NH4Cl, brine
5. dry with materialdried over Na2SO4
6. concentrationConcentration and purification by column chromatography on silica gel (EtOAc:hexane=1:3)