反应详情

温度

80 °C

To a mixture of 2-[2-chloro-5-(trifluoromethyl)phenyl]-1H-pyrrole-3-carbonitrile (450 mg, 1.66 mmol) in toluene (3 mL) was added acetyl chloride (0.176 mL, 2.49 mmol) at room temperature, under nitrogen, and zinc (217 mg, 3.32 mmol). The mixture was allowed to stir for 3 h at 80° C. The mixture was cooled to room temperature, diluted with EtOAc and washed with water. The aqueous layer was separated and extracted twice with EtOAc. The combined organic extracts were washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The crude material was chromatographed on silica gel (0 to 10% EtOAc/hexane) to afford the title compound (386 mg, 74%).

1. temperatureThe mixture was cooled to room temperature
2. washwashed with water
3. customThe aqueous layer was separated
4. extractionextracted twice with EtOAc
5. washThe combined organic extracts were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated under reduced pressure
8. customThe crude material was chromatographed on silica gel (0 to 10% EtOAc/hexane)