反应详情

温度

80 °C

To a solution of 1-(3-bromophenyl)-2-(1H-pyrrol-3-yl)ethane-1,2-dione (93 mg, 0.33 mmol) in DMF (5.0 mL) was added 2,2,2-trifluoroethyl 4-methylbenzenesulfonate (170 mg, 0.66 mmol), K2CO3 (100 mg, 0.73 mmol) and Et4NCl (5.5 mg, 0.033 mmol) at room temperature. After heating at 80° C. for 3 days, the reaction mixture is cooled, diluted with H2O, EtOAc. The two layers are separated and the aqueous layer is extracted with EtOAc. The combined organic extracts are washed with 1N HCl aqueous H2O, brine, dried (MgSO4) and concentrated. The crude material is purified by chromatography (silica gel, EtOAc/hexane: 20/80) to give the title compound (190 mg, 65%) as a solid. mp: 105-106° C. MS (+) ES: 418 (M+CH3COO)−.

1. temperaturethe reaction mixture is cooled
2. customThe two layers are separated
3. extractionthe aqueous layer is extracted with EtOAc
4. washThe combined organic extracts are washed with 1N HCl aqueous H2O, brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customThe crude material is purified by chromatography (silica gel, EtOAc/hexane: 20/80)