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本文报道RCCl_3型化合物的亚磺化脱卤反应.在温和的条件下,四氯化碳及1,1,1-三氯多氟烷烃RCCl_3(R=Cl,F,CF_3,Cl(CF_2)_n,n=2,4,6,8)与连二亚硫酸钠反应,得到亚磺化脱氯产物RCCl_2SO_2Na,产率最高达85％以上.反应在水-乙腈或水-乙醇溶剂中以及碳酸氢钠或碳酸钠存在下进行.反应的最佳温度为25℃左右,提高反应温度,则脱氯氢化成为主要反应.三氯溴甲烷和三氯碘甲烷的亚磺化反应分别生成脱溴及脱碘产物,三氯甲基亚磺酸钠(CCl_3SO_2Na),产率80％左右.RCCl_3型化合物的亚磺化脱卤反应,提供了合成三氯甲基亚磺酸、磺酸及其衍生物的一种新方法,并首次应用于合成α,α-二氯多氟烷基亚磺酸、磺酸等类化合物.
In this paper, the sulfonation and dehalogenation of RCCl 3 -type compounds are reported. Under mild conditions, carbon tetrachloride and 1,1,1-trichlorofluoroparaffins RCCl 3 (R = Cl, F, CF 3, Cl , n = 2,4,6,8) was reacted with sodium dithionite to obtain the sulfonated dechlorination product RCCl_2SO_2Na with a yield up to 85%. The reaction was carried out in water-acetonitrile or water-ethanol solvent and sodium bicarbonate or Sodium carbonate in the presence of the best reaction temperature is about 25 ° C to increase the reaction temperature, the dechlorination hydrogenation as the main reaction trichlorobromomethane and trichloro methyl iodide sulfonation were generated de-bromination and deiodination products, respectively, Trichloromethyl sulfinate (CCl_3SO_2Na), the yield of about 80% .RCCl_3-type compounds sulfonation dehalogenation reaction, the synthesis of trichloromethyl sulfinic acid, sulfonic acid and its derivatives of a new Method, and for the first time applied to the synthesis of α, α-dichloro-polyfluoroalkylsulfinic acid, sulfonic acid and other compounds.