中间体对乙烯基苯磺酰氯的合成研究

Synthesis of p-Vinylbenzenesulfonyl Chloride Intermediate

在低温条件下,以N,N-二甲基甲酰胺为溶剂,以对苯乙烯磺酸钠为原料,合成了对乙烯基苯磺酰氯。分别对反应温度、反应物物质的量比和反应时间进行了优化,采用IR、1 H NMR对产物进行了结构分析,并通过HPLC进行了纯度分析。结果表明,反应温度为1.5℃、对苯乙烯磺酸钠和氯化亚砜的物质的量比为1∶7、反应时间为15min时,产品收率达到96.0%,含量可达93.0%(HPLC)。

p-Vinylbenzenesulfonyl chloride was synthesized from sodium 4-vinylbenzenesulphonate in N,Ndimethylformamide under low temperature.The reaction temperature,molar ratio of reactants and reaction time were optimized.The target compound was characterized by IR and 1 H NMR.The purity was analyzed by HPLC.The results showed that the yield of product reached 96.0% under the optimized conditions,i.e.,the reaction temperature was 1.5 ℃,n（sodium 4-vinylbenzenesulphonate）∶n（thionyl chloride）= 1∶7,and the reaction time was 15 min.The purity was 93.0% by HPLC analysis.