反应详情

To a solution of 2-chloro-3-(2,5-difluorophenyl)thiophene (0.73 g, 3.2 mmol) in CH2Cl2 (100 mL), cooled on ice, chlorosulfonic acid (0.37 g, 3.2 mmol) in CH2Cl2 (50 mL) was added dropwise over 1 h. The reaction was refluxed over night. The reaction mixture was cooled and washed with water (2×100 mL) and brine, dried over MgSO4, filtered and concentrated to a dark brown oil. The oil was dissolved in heptane (50 mL) and stored in the fridge over the weekend. A black tar precipitated. The solution was decanted and concentrated to give the title compound as a light brown oil (0.87 g, 21% over two steps). MS (ESI+) m/z 293 [M−Cl]+.

1. additionwas added dropwise over 1 h
2. temperatureThe reaction was refluxed over night
3. temperatureThe reaction mixture was cooled
4. washwashed with water (2×100 mL) and brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated to a dark brown oil
8. dissolutionThe oil was dissolved in heptane (50 mL)
9. customA black tar precipitated
10. customThe solution was decanted
11. concentrationconcentrated