反应详情

Triethylamine (13.9 g, 137 mmol) was added to a stirred solution of 4-(pentafluoro-λ6-sulfanyl)aniline (Commercially available, for example from Apollo Scientific, Stockport, UK, 10.0 g, 45.6 mmol) in DCM (100 mL) at 0° C. and the mixture was stirred for 15 mins. 2-Chloro-2-oxoethyl acetate (7.47 g, 54.7 mmol) was added at 0° C., and the temperature was raised to room temperature with stirring continued for 4 hr. The reaction mixture was diluted with DCM and washed with ice water, saturated aq NaHCO3 solution and brine solution, dried over anhydrous Na2SO4, and concentrated under reduced pressure to give the crude product. This was purified by recrystallisation from ether (500 mL) to give the title compound (8.64 g).

1. stirringwith stirring
2. waitcontinued for 4 hr
3. washwashed with ice water, saturated aq NaHCO3 solution and brine solution
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated under reduced pressure
6. customto give the crude product
7. customThis was purified by recrystallisation from ether (500 mL)