反应详情

温度

60 °C

A solution of 25.7 g (120 mmol) 2-bromo-1-fluoro-4-nitrobenzene in 154 ml DMF is treated with 10.6 g (150 mmol) sodium thiomethylate and stirred for 5 hours at 60° C. The mixture is stirred at room temperature for 18 hours, again treated with 1.0 g sodium thiomethylate and stirred for a further 6 hours at 60° C. After cooling, the mixture is poured into ice-water and extracted with ethyl acetate (3×). The combined organic phases are washed with water, dried (Na2SO4), filtered and concentrated. The residue obtained is chromatographically purified (hexane/ethyl acetate 2:1). 20.4 g (82 mmol, corresponding to 70% of theor.) of the product is obtained.

1. stirringThe mixture is stirred at room temperature for 18 hours
2. stirringstirred for a further 6 hours at 60° C
3. temperatureAfter cooling
4. extractionextracted with ethyl acetate (3×)
5. washThe combined organic phases are washed with water
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue obtained
10. customis chromatographically purified (hexane/ethyl acetate 2:1)
11. custom20.4 g (82 mmol, corresponding to 70% of theor.) of the product is obtained