二硫化二苯并噻唑的催化合成

Catalytic synthesis of 2,2'-dibenzothiazole disulfide

以2-巯基苯并噻唑和氨水为原料,双氧水作氧化剂,经催化剂A进行催化,合成了二硫化二苯并噻唑。通过考察催化剂种类、催化剂用量、氨水用量、物料配比、反应时间和反应温度对产率的影响,得出适宜的工艺条件为：选用催化剂A,用量为2-巯基苯并噻唑的1%,氨的加入量为n（2-巯基苯并噻唑）∶n（氨水）=1∶6.0,双氧水用量为n（2-巯基苯并噻唑）∶n（双氧水）=2∶1.2,反应时间3 h,反应温度50℃。在此条件下,二硫化二苯并噻唑的产率为90.7%,熔点为165.3~168.7℃。二硫化二苯并噻唑粗品通过甲苯进行一次重结晶后,熔点可达173.6~175℃。

The 2,2＇-dibenzothiazyl disulfide（accelerator DM） was synthesized with 2-mercapto benzothiazole（accelerator M） and ammonia water as materials,hydrogen peroxide as oxidant,and catalyzed with catalyzer A.The effect of the kinds of catalyst,the quantity of the catalyst,the ammonia water,the mass ratio,reaction time and reaction temperature on yield were discussed.The optimal reaction conditions were established as follows：the quantity of the catalyst A was 1% of the accelerator M,n（accelerator M）∶n（ammonia water）=1∶6.0,n（accelerator M）∶n（H2O2）=2∶1.2,reaction time was 3 h and reaction temperature was 50 ℃.Under above conditions,the yield of accelerator DM was 90.7% and the melting point was 165.3~168.7 ℃.After the crude product was recrystallized by toluene,the melting point was 173.6~175 ℃.