反应详情

温度

130 °C

A mixture of 3,4-difluoronitrobenzene (10 g, 62.9 mmol) and sodium methanesulfinate (8.3 g, 69.1 mmol) in DMSO (60 mL) was heated at 130° C. for 8 hours. After cooling down to room temperature, the mixture was poured into ice-water. The whole was extracted with ethyl acetate (200 mL×2), the combined organic layer washed with water (80 mL), brine (80 mL), dried over MgSO4, and concentrated in vacuo. The residue was crystallized from hexane and triturated withhexane to give the subtitle compound (10.2 g, 74% yield).

1. temperatureAfter cooling down to room temperature
2. extractionThe whole was extracted with ethyl acetate (200 mL×2)
3. washthe combined organic layer washed with water (80 mL), brine (80 mL)
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was crystallized from hexane
7. customtriturated withhexane