【摘要】 报道了以芳磺酰胺为起始原料,与氢氧化钾在N,N-二甲基甲酰胺中混合,滴加二硫化碳,在氮气保护下于45°C反应7.5 h,析出棕黄色二硫代芳磺酰亚胺钾盐。过滤,真空干燥,将所得化合物悬浮于无水二氯乙烷中,滴加二(三氯甲基)碳酸酯二氯乙烷溶液,1.5 h加毕,在45°C下持续反应15 h,得芳磺酰异硫氰酸酯,产率61%~75%。更多还原

【Abstract】 An efficient and safe procedure for the synthesis of arylsulfonylisothiocyanates from readily available aryl sulfonamides and bis(trichloromethyl) carbonate(BTC) was introduced.Aryl sulfonamides and potassium hydroxide were mixed in N,N-dimethylformamide(DMF) and carbon disulfide was added dropwise.The reaction mixture was kept under an atmosphere of nitrogen at 45(°C) for 7.5 h,after which brown potassium aryl sulfonyliminodithiocarbonates were precipitated.Following filtration and vacuum drying,the above salts were suspended in anhydrous dichloroethane,and then a solution of BTC in dichloroethane was added dropwise,and the reaction was continued at 45(°C) for 15 h.The arylsulfonylisothiocynates were obtained in 61%~75% yield.更多还原