芳磺酰异硫氰酸酯的合成工艺研究

A Facile Synthesis of Arylsulfonylisothiocynates from Aryl Sulfonamides and Bis(trichloromethyl) Carbonate

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℃反应7.5h，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，1.5h加毕，在45℃下持续反应15h，得芳磺酰异硫氰酸酯，产率61％－75％。

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℃ 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℃ for 15 h. The arylsulfonylisothiocynates were obtained in 61-75% yield.