反应详情

温度

60 °C

To a dimethyl sulfoxide (100 mL) solution of 5-nitro-2-thiophenecarbonitrile (6.30 g, 40.9 mmol) were added p-cresol (8.85 g, 81.8 mmol) and potassium carbonate (11.3 g, 81.8 mmol) under nitrogen atmosphere, which was stirred for 5 hours at 60° C. The reaction solution was cooled to room temperature, and extracted with ethyl acetate after addition of water. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:3→2:1) to obtain the title compound (6.95 g, 78.9%).

1. temperatureThe reaction solution was cooled to room temperature
2. extractionextracted with ethyl acetate
3. additionafter addition of water
4. washThe organic layer was washed with saturated aqueous sodium chloride
5. customthe solvent was evaporated under a reduced pressure
6. customThe residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:3→2:1)