摘要
为制得高品质医药中间体二硫化二苯并噻唑(DM),采用环境友好型氧化剂H2O2和有机溶剂,将二巯基苯并噻唑(M)一步氧化得到DM。通过对反应时间、反应温度、物料配比等因素进行考察,最终得到最佳工艺条件:温度40℃,加料时间1 h,反应时间3 h,碳酸钠5%(以M重量为基准),n(M)∶n(H2O2)=2∶1.1,有机溶剂3倍(以M重量为基准)。在此条件下,DM的熔点可达185℃,纯度高达99%,加入极少量表面活性剂,使最终产率高达96%。
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 time, temperature and the ratio of reactants etc. on reaction results were studied. The obtained optimum reaction conditions were reaction temperature 40℃, dosage of sodium carbonate 5% （ based on M）, the ratio of M to H2O2 2 ： 1.1, the ratio of solvent to M 3 ： 1, addition time 1 h, reaction time 3 h. Under above conditions, the yields was 96% and the purity and melting point of obtained product were 99% and 185℃ respectively.
出处
《青岛科技大学学报（自然科学版）》
CAS
2007年第4期283-286,293,共5页
Journal of Qingdao University of Science and Technology:Natural Science Edition
关键词
过氧化氢
氧化
二硫化二苯并噻唑
hydrogen peroxide
oxidation
dibenzothiazole disulfide
