反应详情

温度

80 °C

A suspension of 1.4 g of a 60% sodium hydride/oil dispersion was prepared in 10 ml of dry DMSO, under an atmosphere of nitrogen. 4-Bromothiophenol (6.5 g) was dissolved in 11 ml of dry DMSO and added slowly to the above suspension. When frothing had subsided 6.0 g of bromomethanesulfonamide was added and the reaction mixture was heated to 80° C. for 2 hours. The reaction mixture was cooled to room temperature and poured into 150 ml of ethyl acetate, filtered from a solid and extracted with brine. The organic phase was dried over anhydrous sodium sulfate and concentrated under vacuum. The resultant residue was recrystallized from toluene to yield 7.9 g (81.4%) of product.

1. additionadded slowly to the above suspension
2. additionwas added
3. temperatureThe reaction mixture was cooled to room temperature
4. filtrationfiltered from a solid
5. extractionextracted with brine
6. dry with materialThe organic phase was dried over anhydrous sodium sulfate
7. concentrationconcentrated under vacuum
8. customThe resultant residue was recrystallized from toluene