反应详情

温度

80 °C

A mixture of 2-[2-(4-bromo-phenyl)-ethanesulfonylamino]-5-methyl-benzenesulfonamide (0.08 g, 0.18 mmol), N,N-diisopropylethylamine (0.1 mL, 0.55 mmol), and copper(I) iodide (7 mg, 0.04 mmol) in anhydrous N,N-dimethylformamide (2 mL) was degassed with nitrogen for 30 min. (1,1′-Bis(diphenylphosphino)ferrocene)-dichloropalladium(II) (14 mg, 0.02 mmol) and 3,3-dimethyl-1-butyne (0.045 mL, 0.37 mmol) were added and the reaction mixture was heated in a sealed tube at 80° C. overnight. The reaction mixture was diluted with ethyl acetate (20 mL), washed with water and brine, dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by preparative TLC, using 5% methanol in dichloromethane as the eluent, to give 20 mg (25% yield) of the title compound.

1. additionwere added
2. washwashed with water and brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by preparative TLC