反应详情

温度

-10 °C

N,N-Diisopropylethylamine (14 μL) is added to a mixture of N-(4-bromobenzenesulfinyl)-2,2,2-trifluoroacetamide (50 mg), N-chlorosuccinimide (25 mg), and dimethylamine solution (2 M in tetrahydrofuran; 0.16 mL) in acetonitrile (2 mL) at −10° C. under an argon atmosphere. The reaction mixture is stirred at −10° C. for 15 min, warmed to room temperature and stirred for 3 h. The reaction mixture is extracted with dichloromethane and the combined extracts are washed with brine, dried over MgSO4, and concentrated in vacuo to give the title compound. The crude product is used for the next step without further purification. LC (method 1): tR=1.07 min; Mass spectrum (ESI+): m/z=359, 361 [M+H]+.

1. temperaturewarmed to room temperature
2. stirringstirred for 3 h
3. extractionThe reaction mixture is extracted with dichloromethane
4. washthe combined extracts are washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo