医药级二硫代二苯并噻唑的合成

Synthesis of medical intermediate dibenzothiazole disulfide

以乙醇水溶液为反应介质,采用环境友好型氧化剂H2O2,将2-巯基苯并噻唑(促进剂M)一步氧化制备高品质医药级二硫代二苯并噻唑(促进剂DM)。考察了反应温度、加料时间、反应时间、溶剂用量、物料配比等因素对反应结果的影响,得到的较佳工艺条件为反应温度35℃,加料时间3h,反应时间3h,V(溶剂)∶m(M)=3.5mL/g,n(M)∶n(H2O2)=2∶1.3。在上述条件下,DM的熔点可达182℃,纯度高达98%,产率高达98%。

Dibenzothiazole disulfide（DM）was prepared using dimercaptobenzothiazole（M）as starting material,H2O2 as oxidizing agent and an organic compound as solvent by one-step method.The effects of factors such as reaction temperature,addition time,reaction time and the ratio of reactants etc.on reaction results were studied.The obtained optimum reaction conditions were reaction temperature35℃,addition time 3h,reaction time 3h,the ratio of solvent to M 3.5∶1,the ratio of M to H2O22∶1.3.Under above conditions,the yield was 98% and the purity and melting point of obtained product were 98% and 182℃respectively.