4-甲基苯亚磺酸钠的合成

Synthesis of Sodium 4-Methylbenzene Sulfinate

研究4-甲基苯磺酰氯为原料还原合成4-甲基苯亚磺酸钠的工艺,以紫外分光光度法分析产物的含量。采用亚硫酸钠水溶液为底物,滴加4-甲基苯磺酰氯的二氯甲烷溶液,反应过程中同时滴加质量分数为10%氢氧化钠水溶液控制pH。最佳工艺条件为:原料配比n(4-甲基苯磺酰氯)∶n(亚硫酸钠)=1∶1.09,反应温度为85℃,反应时间为1h,m(水)/m(4-甲基苯磺酰氯)=10,pH=7.6,收率为89%。

The synthesis of sodium 4-methylbenzene sulfinate was investigated by using the sodium sulfite deoxidization process from the starting material 4-methylbenzene sulfonyl chloride,and the contents of product were analyzed by UV-spectrophotometric method.The aqueous sodium sulfite which used as a substrate was added to dichloromethane solution containing 4-methylbenzene sulfonyl chloride,at the same time,the pH was controlled by adding dropwise 10% sodium hydroxide solution in the reaction process.The optimun reaction conditions were shown as follows：n（4-methylbenzene sulfonyl chloride）∶n（sodium sulfite）=1∶1.09,reaction temperature 85 ℃,reaction time 1 h,m（water）/m（4-methylbenzene sulfonyl chloride）=10,pH=7.6,with a yield of 89%.