杀虫磺的合成新工艺研究

A new process for synthesizing bensultap

研究了由硫化钠与苯磺酰氯反应得到硫代苯磺酸钠盐，再与1-二甲胺基-2，3-二氯丙烷发生亲核取代反应合成目标产物杀虫磺的新工艺．重点对硫代苯磺酸钠盐的反应时间、反应温度和反应溶剂进行了考察，通过正交实验得出最佳合成条件：硫代苯磺酸钠盐的反应温度55～60℃；杀虫磺合成反应时间3h；苯磺酰氯对1-二甲胺基-2，3-二氯丙烷的投料比2：11．2．杀虫磺收率为68％，产品结构经IR，^1H NMR和MS验证．

A new process for synthesizing bensultap by the reaction of 1 dimethylamino-2,3-dichloropropane with sodium benzenethiosulfonate which was prepared by using sodium sulfide and benzenesulfonyl chloride was studied. The factors such as the reaction time, temperature and solvents were investigated. By using an orthogonal design of experiments, optimum synthesis conditions were obtained as follows： the reaction temperature of the sodium benzenethiosulfonate preparation 55-60℃ ,the reaction time for synthesizing bensultap 3 h, and the molar ratio of benzene-sulfonyl chloride to 1-dimethylamino-2,3-dichloropropane 2 ： 1. 2. Under these conditions the yield of bensultap was 68%. The product was analyzcd by IR, ^1H NMR and MS.