反应详情

温度

90 °C

A mixture of 3,4-difluorobenzaldehyde (4.26 g, 30 mmol) and sodium thiomethoxide (2.1 g, 30 mmol) in DMF (40 mL) was heated at 90° C. for 1 hour. After cooling, 2N aqueous HCl was added to the mixture. The whole was extracted with Et2O (70 mL×3), the combined organic layer washed with water, brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash chromatography on silica gel eluting with ethyl acetate/hexane (1/10) to provide the subtitle compound (3.1 g, 61% yield) as a colorless oil.

1. temperatureAfter cooling
2. extractionThe whole was extracted with Et2O (70 mL×3)
3. washthe combined organic layer washed with water, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by flash chromatography on silica gel eluting with ethyl acetate/hexane (1/10)