反应详情

温度

130 °C

A mixture of 2-fluoro-5-nitrobenzotrifluoride (2.09 g, 10 mmol) and sodium methanesulfinate (1.32 g, 11 mmol) in DMSO (20 mL) was heated at 130° C. for 17.5 hours. After cooling down to room temperature, the mixture was poured into ice-water. The whole was extracted with ethyl acetate (30 mL×2), the combined organic layer washed with water, brine, dried over MgSO4, and concentrated in vacuo. The residue was crystallized from hexane to give the subtitle compound (1.56 g, 57.8%, yield).

1. temperatureAfter cooling down to room temperature
2. extractionThe whole was extracted with ethyl acetate (30 mL×2)
3. washthe combined organic layer washed with water, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was crystallized from hexane