反应详情

温度

130 °C

A mixture of 6-fluoro-3′,5′-dimethoxy-4-nitrobiphenyl-3-carbaldehyde (1.7 g, 5.6 mmol) and 4-toluenesulfonic acid (95.8 mg, 0.6 mmol) in 1,2-ethanediol (4.3 mL) and toluene (60 mL) was heated at 130° C. for 3 hours. After that, the reaction mixture was cooled to room temperature, diluted with ethyl acetate (100 mL), and washed by water (100 mL*3) and brine (100 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=8/1 to 5/1) to afford the title compound (1.8 g, 89%) as a yellow solid. MS (ES+) C17H16FNO6 requires: 349, found: 350 [M+H]+.

1. temperatureAfter that, the reaction mixture was cooled to room temperature
2. washwashed by water (100 mL*3) and brine (100 mL)
3. dry with materialThe combined organic layers were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate=8/1 to 5/1)