固体酸催化剂合成吩噻嗪的工艺研究

以二苯胺和硫磺为原料,用固体酸催化剂合成吩噻嗪,讨论反应温度、不同的固体酸催化剂、固体酸催化剂用量、反应物摩尔比、反应时间对合成反应的影响。在优化的合成工艺条件下,以二苯胺与硫磺的摩尔比为1.00∶1.25、固体酸催化剂的质量为二苯胺质量的25.0%、反应时间6 h,纯化后可得吩噻嗪化合物;其产率为83.9%,纯度为99.6%(HPLC)。对产物进行了熔点、TG(thermogravimetric)测试及IR、NMR表征。

Research on the synthesis of phenothiazine catalyzed by solid acid catalyst

Synthesis of phenothiazine by the reaction of diphenylamine with sulfur in the presence of solid acid catalyst activated by p-toluenesulfonic acid was reported in this paper. The reaction conditions, such as temperature, different solid acid catalyst, catalyst loading, molar ratio of reactants, reaction time were investigated. Under the optimized conditions (the molar ratio of diphenylamine to sulfur is 1.00:1.25, the solid acid catalyst accounts for 25.0wt% of diphenylamine, reaction time is 6 hours), phenothiazine was synthesized in 83.9% yield after purification. Its purity is 99.6% by HPLC. Product was determined and characterized by the melting point, TG, IR, NMR.